反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
(5R)-3-(4-(1,2,5,6-Tetrahydropyridin-4-yl)-3-fluorophenyl)-5-(1,2,3-triazol-1-ylmethyl)-oxazolidin-2-one hydrochloride (380 mg, 1 mM) was suspended in dichloromethane (15 ml), 4-dimethylaminopyridine (305 mg, 2.5 mM) added, and the mixture stirred vigorously for 15 minutes. After cooling to 0° C. under nitrogen, methanesulfonyl chloride (229 mg, 2 mM) was added dropwise, and the mixture stirred 18 hours at ambient temperature. Precipitated solid was removed, and the organic solution concentrated, then purified by chromatography on a 10 g silica Mega Bond Elut® column, eluting with a gradient increasing in polarity from 0 to 5% methanol in dichloromethane. Relevant fractions were combined and evaporated to give the desired product (30 mg). MS (ESP): 422 (MH+) for C18H20FN5O4S
WORKUP
后处理
- stirringthe mixture stirred 18 hours at ambient temperature
- customPrecipitated solid
- customwas removed
- concentrationthe organic solution concentrated
- custompurified by chromatography on a 10 g silica Mega Bond Elut® column
- washeluting with
- temperaturea gradient increasing in polarity from 0 to 5% methanol in dichloromethane
- customevaporated