HRID870059

反应详情

EQUATION

反应方程式

HRID 870059 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of methyl 4-{(1S)-1-[({2,5-dimethyl-4-[4-(trifluoromethyl)benzyl]-3-thienyl}carbonyl)amino]ethyl}benzoate from Example 11, Step 5 (5.68 g, 11.9 mmol) in THF (305 mL) and MeOH (152 mL) was treated with LiOH (1N in water, 35.8 mL, 35.8 mmol) at r.t. for 44 h and at 50° C. for 3.5 h. The solution was allowed to cool to r.t., and 1N HCl was added (38.2 mL, 3.2 eq). 350 mL of volatiles were removed in vacuo, 800 mL of water was added to the residue and the resulting suspension was stirred for 19 h. The solid was collected by filtration, rinsed with water and dried. The desired product was obtained as a white solid. MS (−APCI): m/z 460 (M−1)−.

WORKUP

后处理

  1. custom350 mL of volatiles were removed in vacuo, 800 mL of water
  2. additionwas added to the residue
  3. filtrationThe solid was collected by filtration
  4. washrinsed with water
  5. customdried