HRID965553

反应详情

EQUATION

反应方程式

HRID 965553 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

2.17 g of the compound obtained in EXAMPLE 16 in 30 ml of MeOH and 30 ml of THF are reduced with hydrogen under a pressure of 40 bar for 4 hours at RT, in the presence of 1 g of Raney nickel. The mixture is filtered on Celite and the filtrate is evaporated under vacuum. The residue is chromatographed on silica using DCM and then a DCM/AcOEt mixture (90/10; v/v) as the eluent to give the expected product after crystallization from a DCM/iso ether mixture. m=1.3 g. M.p.=198° C.

WORKUP

后处理

  1. filtrationThe mixture is filtered on Celite
  2. customthe filtrate is evaporated under vacuum
  3. customThe residue is chromatographed on silica