HRID323146

反应详情

EQUATION

反应方程式

HRID 323146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-(2-ethoxycarbonylphenyl)benzamide (493 mg) in tetrahydrofuran (20 ml) was cooled in an ice bath. Lithium aluminum hydride (1M solution in tetrahydrofuran, 2.5 ml) was added dropwise to the solution and the mixture was stirred at the same temperature for 2 hours. Water was slowly added to the solution and resulting mixture was acidified with 1N hydrochloric acid. The solution was extracted with chloroform and the organic solution was washed with water and brine, and dried over magnesium sulfate. The solvent was evaporated in vacuo and the residue was subjected to silica gel column (20 g, 2% methanol in chloroform). The product was solidified with diethyl ether to give 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-(2-hydroxymethylphenyl)benzamide (245 mg) as a white powder.

WORKUP

后处理

  1. customresulting mixture
  2. extractionThe solution was extracted with chloroform
  3. washthe organic solution was washed with water and brine
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated in vacuo