HRID469292

反应详情

EQUATION

反应方程式

HRID 469292 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 21.6 g (59.2 mmol) 3-(1-benzyl-piperidin-4-yl)-7-methoxy-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one and 2.5 g palladium on charcoal (10%) in 300 mL methanol was hydrogenated in a 3 bar hydrogen atmosphere at 50° C. until the reaction was complete. The catalyst was removed by suction filtering and the mother liquor was concentrated by rotary evaporation. The residue was triturated with 150 mL DIPE, suction filtered, washed with 100 mL DIPE and dried at 40° C. in the CAD. 13.2 g of the desired product was obtained.

WORKUP

后处理

  1. customThe catalyst was removed by suction
  2. filtrationfiltering
  3. concentrationthe mother liquor was concentrated by rotary evaporation
  4. customThe residue was triturated with 150 mL DIPE, suction
  5. filtrationfiltered
  6. washwashed with 100 mL DIPE
  7. customdried at 40° C. in the CAD