HRID1060467

反应详情

EQUATION

反应方程式

HRID 1060467 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-(2,6-dichlorobenzoyl)-3-acetyl-4-(2-methoxyphenyl)-L-phenylalanine ethyl ester (0.12 g) in EtOH (5 mL) were added NH2OMe HCl salt (24 mg) and DIEA (60 mg). The mixture was refluxed for 2 h and evaporated. The residue was diluted with EtOAc, washed with 1N HCl, dried, and evaporated. The residue was purified by preparative TLC (silica gel; eluent: EtOAc/hexane 2:1)to give 0.058 g of N-(2,6-dichlorobenzoyl)-3-[1-(methoxyimino)ethyl]-4-(2-methoxyphenyl)-L-phenylalanine ethyl ester. ESMS: m/z 534 (M−H)−.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 2 h
  2. customevaporated
  3. additionThe residue was diluted with EtOAc
  4. washwashed with 1N HCl
  5. customdried
  6. customevaporated
  7. customThe residue was purified by preparative TLC (silica gel