HRID377028

反应详情

EQUATION

反应方程式

HRID 377028 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1-diphenylmethyl-3-morpholinoazetidine (Preparation 1(c)) (18.6 g, 60.4 mmol), palladium hydroxide (2 g), ethanol (200 ml) and 1N aqueous HCl (52 ml) was stirred under an atmosphere of hydrogen at 345 kPa (50 p.s.i.) for 3 days. The catalyst was then removed by filtration and the filtrate evaporated to dryness. Addition of dichloromethane (100 ml) to the residue and trituration gave a solid which was recrystallised from methanol to give the title compound (10.2 g) as a crystalline solid. LRMS m/z=179 (m+1)+.

WORKUP

后处理

  1. customThe catalyst was then removed by filtration
  2. customthe filtrate evaporated to dryness
  3. additionAddition of dichloromethane (100 ml) to the residue and trituration
  4. customgave a solid which
  5. customwas recrystallised from methanol