HRID852525

反应详情

EQUATION

反应方程式

HRID 852525 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 3-bromo-5-(4-chloro-butanoylamino)-benzoic acid methyl ester (D13) (530 mg, 1.6 mmol, 1 equiv) in THF (5 ml) at room temperature was added NaH (60% in mineral oil, 64 mg, 1.7 mmol, 1.1 equiv) and the resulting mixture was stirred at room temperature for 2 h. H2O was then added and the resulting mixture was diluted with AcOEt. The two layers were separated and the organic phase dried over MgSO4 and concentrated in vacuo to give 3-bromo-5-(2-oxo-pyrrolidin-1-yl)-benzoic acid methyl ester (D9a) (361 mg, 76%) as a yellow solid. [M−H]-296.3, RT=2.49.

WORKUP

后处理

  1. customThe two layers were separated
  2. dry with materialthe organic phase dried over MgSO4
  3. concentrationconcentrated in vacuo