HRID597676

反应详情

EQUATION

反应方程式

HRID 597676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-(4-Methoxybenzyl)oxycarbonyloxyimino-2-phenylacetonitrile (1.55 g.) was added to a solution of L-phenylalanine (826 mg.) and triethylamine (0.75 ml.) in a mixture of methanol (10 ml.), dioxane (1.5 ml.) and water (7.5 ml.) at room temperature the resulting mixture was stirred for 2 hours at room temperature. The reaction mixture was concentrated and benzene and a sodium bicarbonate aqueous solution were added to the residue. After shaking the resultant mixture, the aqueous layer was separated from the mixture, washed with ether, acidified with hydrochloric acid and extracted with ethyl acetate. The extract was washed with water, dried and concentrated. N-Hexane was added to the residue, and the precipitated crystals were collected by filtration and dried to give N-(4-methoxybenzyl)oxycarbonyl-L-phenylalanine (1.064 g.), mp 87° to 88° C.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. additionbenzene and a sodium bicarbonate aqueous solution were added to the residue
  3. stirringAfter shaking the resultant mixture
  4. customthe aqueous layer was separated from the mixture
  5. washwashed with ether
  6. extractionextracted with ethyl acetate
  7. washThe extract was washed with water
  8. customdried
  9. concentrationconcentrated
  10. additionN-Hexane was added to the residue
  11. filtrationthe precipitated crystals were collected by filtration
  12. customdried