HRID2066802

反应详情

EQUATION

反应方程式

HRID 2066802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 5-(chloromethyl)-3-(5-chloropyridin-2-yl)-1,3-oxazolidin-2-one (204 mg, INTERMEDIATE 1) and sodium azide (107 mg) was heated to 100° C. in 10 ml of dimethylformamide for 15 h. The sample was then diluted with 100 ml of water and extracted with 100 ml of ethyl acetate (3×). The combined organic layers were washed with water (100 ml) and brine (100 ml). They were then dried over sodium sulfate and concentrated in vacuo to provide 139 mg (67%) of the title compound in >95% purity via LC/MS. Mass spectrum (ESI) 254.0 (M+1).

WORKUP

后处理

  1. extractionextracted with 100 ml of ethyl acetate (3×)
  2. washThe combined organic layers were washed with water (100 ml) and brine (100 ml)
  3. dry with materialThey were then dried over sodium sulfate
  4. concentrationconcentrated in vacuo