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Design a college chemical synthesis experiment, including experimental principle, experimental purpose, experimental operation, instruments, drugs, devices and thinking problems.
(Experiment 1) Safety knowledge lecture, glass instrument claim 1, experiment purpose requirement (1) Understand the general safety knowledge of organic chemistry experiment and the rules of organic chemistry laboratory; (2) Understand the requirements of organic chemistry experiment course (including experiment discipline, experiment report, preview, experiment record, experiment redo requirements) (3) Experiment is an important link to cultivate independent work and thinking ability, and must be completed independently. 2. Main contents of the experiment (1) Explanation of basic experimental knowledge (2) Explanation of safety knowledge (3) Claim of experimental instruments (4) Washing of experimental instruments (1) Enter the laboratory on time, listen carefully to the instructor to explain the experiment and answer questions. Difficult questions should be put forward in time and prepared for the experiment under the guidance of the teacher. (2) After the experimental instruments and devices are assembled, they must be checked and approved by the instructor before they can be connected to the power supply for experiments. Experimental operation and instrument use should be carried out in strict accordance with the operating procedures. (3) During the experiment, we should concentrate our efforts, carefully observe the experimental phenomena, record the experimental data realistically, think positively, find out the reasons for the abnormal phenomena seriously, or ask the instructor to help us analyze and deal with them. Experimental records are the first-hand data of scientific research, and the quality of experimental records directly affects the analysis of experimental results. Therefore, the whole process of the experiment must be carefully observed and recorded, especially the following contents: ① The amount, order and color of the added raw materials. (2) With the increase of temperature, the color of the reaction solution changes, and there is no precipitation or gas. (3) The data of product quantity and color, melting point, boiling point and refraction shall be recorded in time and truly. When recording, it should correspond to the operation one by one, the content should be concise and accurate, and the handwriting should be clear. 3. Discuss the topic in class 1, and how to write the preview report 4. Topic selection 1, how to observe and record the whole process of the experiment carefully, 2. (Experiment 2) Synthesis of 1- bromobutane (nucleophilic substitution reaction) 1, experimental purpose requires 1, master (Experiment 2) 2. Understand reversible reaction and equilibrium motion; 3. Master the synthesis method of low boiling point volatile organic compounds. 4. Understand the principle and method of preparing 1- bromobutane from sodium bromide, concentrated sulfuric acid and n-butanol. 2. The main content of the experiment is 1. Performing reflux heating operation with a device for absorbing harmful gases; 2. Distillation and reflux (with gas absorption device); 3. Normal temperature filtration and thermal filtration technology; 4. Washing and drying of liquid organic matter. 3, class discussion topic 1, how to absorb harmful gases in the experiment? 4. What are the factors that affect the response of SN 1 and SN2? 3. (Experiment 3) Synthesis of ether (dehydration reaction) 1, experimental purpose 1, and master the basic methods of ordinary distillation, boiling point and refractive index determination; 2, master the principle and method of preparing ether in the laboratory; 3, master the distillation operation of low boiling point flammable liquid. 2. The main contents of the experiment are 1, constant method and micro method to determine the boiling point of liquid organic matter; 2. Use a separating funnel and a dropping funnel; 3. Distillation of flammable liquid with low boiling point; 24. Ether separation. 3. Class discussion topic 1. How to collect organic compounds with low boiling point in experiments? 4, homework topic 1, the preparation principle and method of simple ether? 4. (Experiment 4) Synthesis of n-butyl ether (dehydration reaction) 1, experimental purpose requirements 1, mastering the basic methods of ordinary distillation and determination of boiling point and refractive index; 2. Master the principle and method of preparing n-butyl ether in the laboratory; 3, master the use of oil-water separator and experimental operation. 4, master the distillation operation of flammable liquid. 2. The main content of the experiment is 1. The oil-water separator 2 refluxes to prepare n-butyl ether. Drying, washing and distillation of n-butyl ether. 3. Use a separating funnel and a dropping funnel. 3. Class discussion topic 1. Why do you use an oil-water separator in the experiment? 4, homework topic 1, preparation principle and method of mixed ether? 5. (Experiment 5) Synthesis of methyl orange (diazotization reaction) 1, experimental purpose requirements 1, mastering the basic principles of ordinary distillation, boiling point and optical rotation determination; 2. Through the preparation of methyl orange, master the principle and method of diazotization and even nitridation; 3. Consolidate the principle and operation of salting-out and recrystallization. 4, further familiar with the purification method of solid organic compounds. 2. The main contents of the experiment are 1, synthesis, crystallization, washing and recrystallization of methyl orange 2, decoloration of methyl orange 3, drying of solid 4, purification of methyl orange 3, 1. How to decolor and purify methyl orange in the experiment is discussed in class. 4. Homework topic 1. Principles and methods of diazotization reaction and even nitridation reaction? Intransitive verb (experiment 6) Synthesis of isoamyl acetate (esterification) 1. The experimental target needs 1. Proficient in the principle and method of preparing carboxylate by direct esterification under acid catalysis. 3. Master the reflux method to synthesize organic compounds. 3. Master the selection and drying method of ethyl acetate liquid desiccant. 2. The main content of the experiment is 1. Synthesis of isoamyl acetate by reflux under acid catalysis. 2. Use a separating funnel and a dropping funnel 3. Drying of isoamyl acetate solution. Separation of crude products. 3. Class discussion topic 1. How to wash and separate isoamyl acetate in the experiment? 4, homework topic 1, the principle and side effects of esterification? Seven. (Experiment 7) Synthesis of cyclohexene (dehydration reaction) 1, and the experimental purpose requires 1 to understand the basic principle of elimination reaction; 2. Learn the principle and active method of preparing cyclohexene by dehydration of cyclohexanol catalyzed by concentrated phosphoric acid; 3. Master the basic operations of fractionation and water bath distillation; 2. Main contents of the experiment: 1. Catalytic dehydration of cyclohexanol to cyclohexene by concentrated phosphoric acid; 2. Washing, drying and distilling cyclohexene; 3. Qualitative analysis of the sample by refraction method. 3. The topic discussed in class is 1, the use of fractionator in the experiment and the basic operation of water bath distillation. 4. The homework topic is 1. What are the basic principles and methods of fractionation? Eight. (Experiment 8) Synthesis (oxidation reaction) of cyclohexanone 1, the experimental purpose requires 1, and learn the principle and method of preparing cyclohexanone by oxidation; 2. A method for converting a secondary alcohol into a ketone; 3. Further understand the difference between alcohol and ketone. 2. The main content of the experiment is 1. Oxidizing cyclohexanol with strong oxidant to generate cyclohexanone; 2, using a stirring device to separate products; 3. Purification and infrared spectrum determination of the product. 3. Class discussion topic 1. Basic operation of stirring in product experiment and purification? 4, homework topic 1, the basic principle and method of oxidation reaction? Nine. (Experiment 9) Synthesis of adipic acid (oxidation reaction) 1, and the purpose of the experiment requires 1 to understand the principle, application and influencing factors of oxidation reaction; 2. Master the method of converting secondary alcohol into dibasic acid by strong oxidant; 3. Master the operation methods such as concentration, filtration and recrystallization. 2. The main content of the experiment is 1. Oxidizing cyclohexanol with potassium permanganate to generate adipic acid; 42, recrystallization separation of adipic acid; 3. Drying of adipic acid and determination of its melting point. 3. Class discussion topic 1. Basic operation of electromagnetic stirring in experiment and product purification? 4, homework topic 1, the basic principle and method of measuring melting point? X. (Experiment 10) Synthesis of Furanoformic Acid and Furanomethanol (disproportionation reaction) 1. The purpose of the experiment requires 1. Master the principle and experimental method of disproportionation reaction; 2. Master the conditions of disproportionation reaction and redox reaction of aldehyde without α-H catalyzed by strong alkali. 3. Understand redox reaction and equilibrium movement; 4. Master the synthesis and separation methods of organic acids and alcohols. 2. The main content of the experiment: 1, synthesis of furoic acid and furfuryl alcohol from aldehyde without α-H catalyzed by strong base; 2. Extraction and separation of furoic acid and furfuryl alcohol. 3. Washing and drying of liquid organic matter. Acidification of furoic acid and purification of solid matter. 3. The topic discussed in class is 1, the principle and experimental method of disproportionation reaction 4. The homework topic is 1, what are the conditions of disproportionation reaction? XI。 (Experiment 1 1) Synthesis of acetanilide (acylation reaction) 1, experimental purpose requirements 1, mastering the basic principles of ordinary distillation, boiling point and optical rotation determination; 2. Master the application of arylamine acylation, the principle and experimental operation of aniline acetylation, 3. Learn more about the purification methods of solid organic compounds. 2. The main contents of the experiment are 1, the use of fractionator, crystallization, washing and recrystallization. 2. Master the principle and method of thermal filtration. 3. Dry the solid. 4. Decolorization of acetanilide. 3. The topic discussed in class is 1, the principle and experimental method of arylamine acylation 4. The homework topic is 1, the principle and method of thermal filtration? Twelve. (Experiment 12) Synthesis and content determination of aspirin 1. The purpose of the experiment requires 1. Master the basic principle of spectral determination; 2. Master the principle and method of esterification reaction through the preparation of acetylsalicylic acid; 3. Learn the method of synthesizing aspirin by esterification of salicylic acid and acetic anhydride. 4, further familiar with the purification method of solid organic compounds. 2. The main content of the experiment is 1, synthesis, crystallization, washing and recrystallization of aspirin; 2. Use a separating funnel and a dropping funnel; 3. Purification of acetylsalicylic acid by salting-out and recrystallization: 4. Decolorization of aspirin. 5. Analytical titration of aspirin. Spectral analysis method of aspirin. 57. Qualitative and quantitative determination of aspirin by HPLC. 3. Class discussion topic 1 Principle and experimental method of esterification of salicylic acid and acetic anhydride to synthesize aspirin 4. Topics in homework 1. How to determine aspirin qualitatively and quantitatively by HPLC? Thirteen. (Experiment 13) Design of synthesis method, content determination and spectral determination of furacrylic acid. (condensation reaction) 1, the experimental purpose requires 1, consult relevant literature, design and determine feasible semi-micro or micro experimental scheme; 2. Master the aldol condensation reaction of aromatic aldehyde and anhydride under the action of alkaline catalyst to generate α, β-unsaturated aromatic aldehyde; 3. Understand the structure, physical and chemical properties and uses of furacrylic acid, as well as the physical and chemical properties of reactants, and consult relevant information to design the experimental route; 4. Understand what other synthetic methods are available, and clarify the toxicity of chemical reagents needed for the experiment and the key points of protective treatment; 5. Prepare the experiment after the design route is approved by the teacher; 6. Consolidate the principle and operation of salting-out and recrystallization. 7. Qualitative and quantitative determination of furacrylic acid by HPLC. 2. The main contents of the experiment are 1, synthesis, crystallization, washing and recrystallization of furacrylic acid 2, use of separating funnel and dropping funnel 3, decoloration, washing, drying and recrystallization of solid 4, separation of furacrylic acid. 5. Spectral analysis of furan acrylic acid. 6. Qualitative and quantitative determination of furacrylic acid by HPLC. 3. Class discussion topic 1, aldol condensation reaction principle and experimental method of aromatic aldehyde and anhydride under the action of alkaline catalyst 4. After-class homework topic 1, how to determine furacrylic acid qualitatively and quantitatively by HPLC. The examination contents include: 1, design of experimental method 2, query of experimental data 3, basic operation 4, record 5, calculation of output 6, experimental report 1, and general principles of performance evaluation: teachers' preparation for students before class, equipment, operation process, basic operation, experimental safety, product quantity and quality, experimental report, scientific attitude, etc. Pay attention to correct some existing problems in time, mainly based on each experimental result (85 ~ 90%) and experimental report (10 ~ 15%), with an average at the end of the period. Among the total grades, the usual grades account for 60%, and the final exam accounts for 40%. 2. The usual performance evaluation is mainly based on the experimental results (85 ~ 90%) and experimental reports (10 ~ 15%), and the average results are obtained at the end of the period. 3. Final assessment Two final exams can be arranged in a comprehensive experiment (one of which is operated independently by one person), one can be arranged as a written exam, and the other is a comprehensive experimental exam operated independently by one person.