HRID1264092

反应详情

EQUATION

反应方程式

HRID 1264092 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred, partial solution of 4-[4-(4-methyl-benzoylamino)-phenyl]-4-oxo-butyric acid, methyl ester (0.5748 g, 0.00177 mol) in THF (11 mL) was added 1.0 M NaOH (3.7 mL, 0.0037 mol), and the mixture was stirred overnight. The resulting suspension was filtered, and the filtercake was washed with THF. The solids were partitioned between EtOAc-THF and 0.2 M HCl, and left for 8 days. The solids were filtered, washed with water, and dried in vacuo to give 0.2133 g of 4-[4-(4-methyl-benzoylamino)-phenyl]-4-oxo-butyric acid as an off-white solid; mp 257-258° C.

WORKUP

后处理

  1. filtrationThe resulting suspension was filtered
  2. washthe filtercake was washed with THF
  3. customThe solids were partitioned between EtOAc-THF and 0.2 M HCl
  4. waitleft for 8 days
  5. filtrationThe solids were filtered
  6. washwashed with water
  7. customdried in vacuo