HRID77001

反应详情

EQUATION

反应方程式

HRID 77001 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of [(4-fluoro-phenyl)-methyl-amino]-phenyl-acetic acid ethyl ester (I70) (0.59 g, 2.05 mmol) in THF (10 mL) and water (10 mL), is added lithium hydroxide hydrate (0.26 g, 6.14 mmol). The reaction is stirred at RT for 3.5 hours and then at 70° C. for 24 hours. 3N HCl is added till pH is about 1 and the mixture is evaporated. Water (15 mL) is added and the residue is triturated obtaining a pale brown suspension that is filtered on a buckner funnel, washed with water and then with acetonitrile. The solid is dried under vacuum at 40° C. overnight to obtain intermediate I119 as a pale brown powder (0.44 g, 72% yield).

WORKUP

后处理

  1. waitat 70° C. for 24 hours
  2. customthe mixture is evaporated
  3. additionWater (15 mL) is added
  4. customthe residue is triturated
  5. customobtaining a pale brown suspension that
  6. filtrationis filtered on a buckner funnel
  7. washwashed with water
  8. customThe solid is dried under vacuum at 40° C. overnight