2 (6.3 mg, 0.02 mmol) dissolved, [bmim] pf6 (0.5 ml).
And methanol (3.2 ml) in a 20 ml ampoule. Sulfide (1 mmol)
Followed by hydrogen peroxide (30%, water) (170
L). Stir the reaction for a given time (reaction
Followed by thin layer chromatography) to remove methanol.
The residual ionic liquid was extracted with ether (3 15ml). Treating sodium in combination with ether layer
Lotus seed and water washing (3 10 ml). Ether stage
Drying with sodium sulfate, filtering, and vacuum concentrating. that
Product purification routine or biotage rapid chromatography.
1 hr, and then p-tolylmethyl sulfoxide is isolated (Article 8 B).
Reaction time, 78%. Nuclear magnetic resonance data show that.
The previously reported .4 transformation (Figure 3) determines that
The reaction mixture was analyzed by gas chromatography: TR (tolylmethyl sulfide).
) 12.7 minutes; TR (tolyl methyl sulfoxide)) 17.2 minutes.
The general procedure is to recover ionic liquid.
Catalyst system. Catalyst precursor 2 (6.3 mg 0.02 mmol)
Dissolved in [bmim] pf6 (0.5) and methanol (3.2 ml).
20 ml ampoule. Sulfide (1 mmol) was expressed at that time, and then
Hydrogen peroxide (170L). After a given time, the reaction (reaction, followed by thin layer chromatography) is stirred, in which methanol
And diethyl ester is extracted from the remaining ionic liquid.
Alkaline ether (315ml). Combined ether layer therapy
Sodium hydrosulfite and water washing (10ml). aqueous phase
Extract with ether (3 10 ml). merge
The ether stage was dried with sodium sulfate, filtered and concentrated.
Vacuum. The product was isolated by flash chromatography. that
After the ionic liquid phase, it is evaporated, while the rest
Ether. Adding sulfide (1 mmol) and hydrogen peroxide (1.5 equivalent);
After that, except methanol (3.2 ml).