HRID747207

反应详情

EQUATION

反应方程式

HRID 747207 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(5R)-5-(Azidomethyl)-3-(4-Iodophenyl)-1,3-oxazolidin-2-one (8.0 g, 23.2 mmol) was dissolved in acetonitrile (160 ml) and water (16 ml). Triphenylphosphine (7.3 g, 27.9 mmol) was added and the mixture stirred at room temperature overnight. The volatiles were removed by concentration in vacuo, and the resulting residue partitioned between water (200 ml) and dichloromethane (200 ml). The aqueous layer was extracted with dichloromethane (2×200 ml) and dried over sodium sulfate. The crude material was purified by flash chromatography on silica gel with 0-10% methanol in dichloromethane as the eluent giving the desired product (6.0 g).

WORKUP

后处理

  1. customThe volatiles were removed by concentration in vacuo
  2. customthe resulting residue partitioned between water (200 ml) and dichloromethane (200 ml)
  3. extractionThe aqueous layer was extracted with dichloromethane (2×200 ml)
  4. dry with materialdried over sodium sulfate
  5. customThe crude material was purified by flash chromatography on silica gel with 0-10% methanol in dichloromethane as the eluent