HRID1713088

反应详情

EQUATION

反应方程式

HRID 1713088 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

7-Methoxy-3-(toluene-4-sulfonyl)-2,3,4,5-tetrahydro-benzo[d]azepin-1-one (6.91 g, 20 mmol) (prepared essentially as described by Kanao et al. (1982) Chem. Pharm. Bull. 30:180-88) is added to a mixture of acetic acid (20 ml), 37% hydrochloric acid (8 ml), EtOH (8 ml) and dioxane (80 ml). 1.0 g of 10% palladium-carbon is added to the mixture, and the resulting mixture is hydrogenated under 30-55 psi at rt overnight. The palladium-carbon is removed by filtration, and the filtering cake is washed with MeOH (30 ml×3). The combined organic phase is evaporated to dryness under reduced pressure to give the title compound as a white solid. MS (+VE) m/z 332.1 (M+).

WORKUP

后处理

  1. customThe palladium-carbon is removed by filtration
  2. washthe filtering cake is washed with MeOH (30 ml×3)
  3. customThe combined organic phase is evaporated to dryness under reduced pressure