HRID1733654

反应详情

EQUATION

反应方程式

HRID 1733654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

N-Benzyloxycarbonyl-S-benzyl-L-cysteine (1.73 g) and glycine ethyl ester hydrochloride (0.70 g) are dissolved in dimethylformamide (12 ml), and thereto are added triethylamine (1.40 ml) and further ethyl 2-methanesulfonyloxyimino-2-cyanoacetate (1.1 g). The mixture is allowed to stand at room temperature for 14 hours. To the reaction mixture are added water and ethyl acetate, and the ethyl acetate layer is separated, washed with water, 1 N hydrochloric acid, a saturated aqueous sodium hydrogen carbonate and water in order and then dried over anhydrous magnesium sulfate. After drying, the solvent is distilled off and the resulting residue is crystallized from ethanol-petroleum ether, separated by filtration and dried to give N-(N-benzyloxycarbonyl-S-benzyl-L-cysteinyl)glycine ethyl ester (0.5 g), melting point: 93°-95° C. The product is identified with an authentic sample by infrared spectrum.

WORKUP

后处理

  1. customthe ethyl acetate layer is separated
  2. washwashed with water, 1 N hydrochloric acid
  3. dry with materiala saturated aqueous sodium hydrogen carbonate and water in order and then dried over anhydrous magnesium sulfate
  4. customAfter drying
  5. distillationthe solvent is distilled off
  6. customthe resulting residue is crystallized from ethanol-petroleum ether
  7. customseparated by filtration
  8. customdried