反应详情

温度

0 °C

Methanesulfonyl chloride (1.93 ml, 24.9 mmol) is added to a cooled (0° C.) solution of ((7R,8S)-8-hydroxymethyl-1,4-dioxa-spiro[4.4]non-7-yl)-methanol (Tet. Lett., 2002,43, 4947; 1.17 g, 6.22 mmol) and triethylamine (3.50 ml, 24.9 mmol) in dichloromethane (30 ml). The reaction is stirred for 2 hours at 0° C. and then partitioned between dichloromethane and iced water. The organic phase is washed with 1M aqueous HCl, saturated aqueous NaHCO3, brine, dried (MgSO4) and evaporated to afford methanesulfonic acid (7R,8S)-8-methane-sulfonyloxymethyl-1,4-dioxaspiro[4.4]non-7-ylmethyl ester, MH+345.

1. custompartitioned between dichloromethane and iced water
2. washThe organic phase is washed with 1M aqueous HCl, saturated aqueous NaHCO3, brine
3. dry with materialdried (MgSO4)
4. customevaporated