HRID1733977

反应详情

EQUATION

反应方程式

HRID 1733977 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a slurry of 0.50 g of 6,7,8,9-tetrahydro-9-(4-nitrobenzoyl)-5H-pyrido[2,3-b]azepin-5-one in 10 ml of tetrahydrofuran under argon is added 0.70 g of tert-butoxy-bis(dimethylamino)methane and the mixture is stirred at room temperature overnight. The volatiles are removed under vacuum and the residue in ethyl acetate-CH2Cl2 (2:8) filtered through a short column of silica gel. The silica gel is washed with ethyl acetate (discard) and then with chloroform containing 3% methanol to give 0.51 g of the product as a yellow solid.

WORKUP

后处理

  1. customThe volatiles are removed under vacuum
  2. filtrationthe residue in ethyl acetate-CH2Cl2 (2:8) filtered through a short column of silica gel
  3. washThe silica gel is washed with ethyl acetate (discard)