HRID2035678

反应详情

EQUATION

反应方程式

HRID 2035678 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4-bromo-2-methoxybenzoic acid (950.7 mg, 4.11 mmol) in 8 ml of DMF was treated sequentially with EDC (1183 mg, 6.17 mmol) and HOBT (945 mg, 6.17 mmol) and stirred at room temperature for 10 minutes. The reaction was then treated with acetic hydrazide (366 mg, 4.94 mmol) and stirred at room temperature overnight. The reaction was dissolved in EtOAc and washed sequentially with saturated bicarbonate solution and brine. The aqueous washes were extracted once with EtOAc. Organics were combined, dried over sodium sulfate, and concentrated under reduced pressure to a white solid (1.37 g crude).

WORKUP

后处理

  1. stirringstirred at room temperature overnight
  2. washwashed sequentially with saturated bicarbonate solution and brine
  3. extractionThe aqueous washes were extracted once with EtOAc
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under reduced pressure to a white solid (1.37 g crude)