HRID1107114

反应详情

EQUATION

反应方程式

HRID 1107114 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a solution of 1 g (3.31 mmol) of 3-(4-methoxyphenylsulfanyl)-4-phenylbutyric acid in 30 mL of CH2Cl2 at 25° C. under argon is added 0.2 mL of DMF followed by 4.1 mL (8.27 mmol) of 2 M solution of oxalyl chloride in CH2Cl2. After stirring at 25° C. for 1.5 hours, 2.1 mL (16.53 mmol) of O-trimethylsilylhydroxylamine is added and this is then stirred at 25° C. for 18 hours. The reaction is partitioned between CH2Cl2 and 1 N HCl. The organic layer is dried over anhydrous Na2SO4 and concentrated in vacuo. Purification by flash silica gel chromatography affords 0.86 g (82%) of N-hydroxy-3-(4-methoxyphenylsulfanyl)-4-phenylbutyramide as a yellow crystalline solid.

WORKUP

后处理

  1. stirringthis is then stirred at 25° C. for 18 hours
  2. customThe reaction is partitioned between CH2Cl2 and 1 N HCl
  3. dry with materialThe organic layer is dried over anhydrous Na2SO4
  4. concentrationconcentrated in vacuo
  5. customPurification by flash silica gel chromatography