HRID1453203

反应详情

EQUATION

反应方程式

HRID 1453203 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

An aqueous solution of NaOH (1 M, 270 mL) was added to a mixture of the 3-(4-benzyloxyphenyl)propionic acid methyl ester from Step 2 above in MeOH (600 mL) and the reaction was stirred overnight. The crystalline ppt was collected by filtration, air dried and then partitioned between EtOAc/Et2O/1 M HCl (500 mL, 250 mL, 150 mL). The organic phases were dried over MgSO4 and evaporated to give the product as a white solid (16.2 g, 70%, 3 Steps). 1H NMR (CDCl3) δ 2.61-2.68 (m, 2H), 2.86-2.93 (m, 2H), 5.03 (s, 2H), 6.88-6.93 (m, 2H), 7.10-7.15 (m, 2H), 7.28-7.45 (m, 5H).

WORKUP

后处理

  1. filtrationThe crystalline ppt was collected by filtration, air
  2. customdried
  3. custompartitioned between EtOAc/Et2O/1 M HCl (500 mL, 250 mL, 150 mL)
  4. dry with materialThe organic phases were dried over MgSO4
  5. customevaporated