反应详情

Methylisocyanate (243 mg) was dissolved in anhydrous dichloromethane (5 ml). To the solution were added N-triphenylmethylcysteamine (3.19 g: 0.33 equimolar amount) while cooling with ice. The reaction solution was stirred at room temperature for 4 hours and was concentrated under reduced pressure. The residue was dissolved in chloroform (50 ml), and the chloroform solution was well washed with water and a saturated solution of sodium chloride. Anhydrous sodium sulate was used to dry the chloroform layer which was then concentrated under reduced pressure. The residue was purified by silica gel chromatography using a solvent system of hexane/ethyl acetate (5:1 v/v) to obtain the desired substance (297 mg) with a yield of 79%.

1. temperaturewhile cooling with ice
2. concentrationwas concentrated under reduced pressure
3. dissolutionThe residue was dissolved in chloroform (50 ml)
4. washthe chloroform solution was well washed with water
5. dry with materialto dry the chloroform layer which
6. concentrationwas then concentrated under reduced pressure
7. customThe residue was purified by silica gel chromatography
8. customto obtain the desired substance (297 mg) with a yield of 79%