HRID1060466

反应详情

EQUATION

反应方程式

HRID 1060466 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 (0.15 g) in n-BuOH (5 mL) were added NH2OH HCl salt (23 mg) and NaOAc (40 mg). The mixture was refluxed for 6 hour, then evaporated. The residue was diluted with CH2Cl2, washed with 1N HCl, dried and evaporated. The residue was purified by preparative TLC (silica gel; eluent: EtOAc/hexane 1:1) to give N-(2,6-dichlorobenzoyl)-3-[1-(hydroxyimino)ethyl]-4-(2-methoxyphenyl)-L-phenylalanine ethyl ester. ESMS: m/z 490 (MH+).

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 6 hour
  2. customevaporated
  3. additionThe residue was diluted with CH2Cl2
  4. washwashed with 1N HCl
  5. customdried
  6. customevaporated
  7. customThe residue was purified by preparative TLC (silica gel; eluent: EtOAc/hexane 1:1)