HRID723800

反应详情

EQUATION

反应方程式

HRID 723800 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. stirringthe mixture stirred 18 hours at ambient temperature
  2. customPrecipitated solid
  3. customwas removed
  4. concentrationthe organic solution concentrated
  5. custompurified by chromatography on a 10 g silica Mega Bond Elut® column
  6. washeluting with
  7. temperaturea gradient increasing in polarity from 0 to 5% methanol in dichloromethane
  8. customevaporated