HRID55252

反应详情

EQUATION

反应方程式

HRID 55252 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.55 g of 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine in 8 ml of methylene chloride is added 0.55 g of triethylamine followed by 0.97 g of 3-methoxy-4-nitrobenzoyl chloride. The reaction mixture is stirred at room temperature for 2 hours and then quenched with 10 ml of 1N NaOH. The methylene chloride layer is evaporated and the resulting suspension filtered. The precipitate is washed with 1N NaOH (2×5 ml), water (3×5 ml) and hexane (2×5 ml). The collected solid is dried in vacuo to give 1.13 g of off-white solid. MS (CI): 364(M+H).

WORKUP

后处理

  1. customquenched with 10 ml of 1N NaOH
  2. customThe methylene chloride layer is evaporated
  3. filtrationthe resulting suspension filtered
  4. washThe precipitate is washed with 1N NaOH (2×5 ml), water (3×5 ml) and hexane (2×5 ml)
  5. customThe collected solid is dried in vacuo