First, the purpose of the experiment.

1. Learn the principle and method of preparing 1- bromobutane from sodium bromide, concentrated sulfuric acid and n-butanol.

2, learn to install harmful gas absorption device, consolidate the operation of heating reflux.

Second, experimental supplies.

Drugs: 4 ml concentrated H2SO4, 2.5 ml N-C4 H9OH; ; 3.3g NaBr； Saturated NaHCO3? Solution.

Instrument: semi-micro organic preparation instrument.

25 ml round bottom flask; Spherical condenser tube; Airway; Small glass funnel; 10 ml measuring cylinder; 250 ml beaker; 75 degree bend; Direct condensing tube; Tailpipe; Vacuum plug; Two cylindrical separatory funnels; 2 5 mL round bottom flasks; 30 ml conical flask1; Distillation head; Thermowell; Thermometer (200℃).

Third, experimental methods.

Add 1 and 100ml three-necked bottles, which contain 13.67g sodium bromide and 10ml n-butanol. The flask is equipped with a reflux condenser tube, which can absorb harmful gases.

2. Add 10ml water to the conical flask, and add 16ml sulfuric acid while shaking. Cooling with cold water, adding mixed solution from a three-necked bottle, refluxing zeolite with low fire for 59 minutes, and cooling.

3. Remove the waste gas device, add 30ml ice water to the three-necked bottle, dissolve the solid, pour it into the separating funnel, add 5ml cooled concentrated sulfuric acid to the organic layer, shake well, let stand for layering, and let out the lower layer. The upper layer 1- bromobutane was sequentially used with 8 ml of saturated sodium carbonate, and the lower layer was collected. Then wash with 10ml water, and collect the lower layer. After that, it was added into a small conical flask and dried with anhydrous calcium chloride.

4. Then, the crude product was filtered into a 50 ml distillation bottle, distilled with low fire, and fractions were collected.

Fourth, experimental drugs.

1, n-butanol: Tianjin Fengchuan Chemical Reagent Technology Co., Ltd. (AR 20 1009 18).

2. Sodium bromide: Tianjin No.3 Chemical Reagent Factory (AR 200503 10).

3.NAOH: Tianjin Fengchuan Chemical Reagent Technology Co., Ltd. (AR 20 100508).

4. Anhydrous calcium chloride: Tianjin Guangfu Institute of Fine Chemical Industry (AR 20 10 1025).

5. Concentrated sulfuric acid: beijing chemical works (AR 20 100304).

6. Sodium carbonate: Tianjin Fengchuan Chemical Reagent Technology Co., Ltd. (AR 20 100308).

Fifth, matters needing attention.

When the liquid is separated by the separating funnel, the crude product is poured into the separating funnel and the lower layer is discarded (first liquid separation); After adding concentrated sulfuric acid (secondary liquid separation), discard the lower layer; When washing with saturated sodium carbonate and water (third and fourth liquid separation), discard the upper layer.

Sixth, data processing.

1, mass of sodium bromide:13.67g.

2. Start time of the reaction: 14:39 and end time: 15: 38.

3. Distillation start time: 16. 10 end time: 16.28.

4. Boiling point range: 99- 100℃.

5. Bottle weight:17.08g Bottle+product weight: 24.09g.