反应详情

温度

0 °C

A solution of [1-({[tert-butyl(dimethyl)silyl]oxy}methyl)cyclopropyl]methanol (Example 34c, 5.37 g) dissolved in DCM (20 mL) was treated with triethylamine (6.92 mL) at 0° C. before adding methanesulfonyl chloride (2.321 mL) under nitrogen. The resulting mixture was stirred at 0° C. for 30 min. The reaction mixture was diluted with water (100 mL), and extracted with DCM (250 mL). The organics were dried (MgSO4), filtered and evaporated. The crude product was purified (SiO2 chromatography, elution 50% isohexane in diethyl ether). Pure fractions were evaporated to dryness to afford the subtitle compound (5.37 g) as an oil.

1. extractionextracted with DCM (250 mL)
2. dry with materialThe organics were dried (MgSO4)
3. filtrationfiltered
4. customevaporated
5. customThe crude product was purified
6. wash(SiO2 chromatography, elution 50% isohexane in diethyl ether)
7. customPure fractions were evaporated to dryness