HRID2249977

反应详情

EQUATION

反应方程式

HRID 2249977 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

D-Phenylalanine methyl ester hydrochloride (20 g, 0.092 mol) was suspended in a solution of triethylamine (66 mL) in dichloroethane (100 mL) and the mixture was stirred for 1 hour at room temperature. The organic layer was separated after washing with water and dried over anhydrous sodium sulphate. Trans-4-isopropylcyclohexane carboxylic acid (15.8 g, 0.092 mol) was added to the organic layer followed by LiOH—Al2O3 (5.5 g of LiOH adsorbed on 40.5 g aluminum oxide) and the resulting mixture heated at for 24 hours. The reaction mixture was filtered through a celite bed and washed with 1.5 N HCl, 5% sodium bicarbonate solution and brine. The organic layer was concentrated to yield 15.5 g of N-(trans-4-isopropylcyclohexylcarbonyl)-D-phenylalanine methyl ester.

WORKUP

后处理

  1. customThe organic layer was separated
  2. washafter washing with water
  3. dry with materialdried over anhydrous sodium sulphate
  4. temperaturethe resulting mixture heated at for 24 hours
  5. filtrationThe reaction mixture was filtered through a celite bed
  6. washwashed with 1.5 N HCl, 5% sodium bicarbonate solution and brine
  7. concentrationThe organic layer was concentrated