HRID17364

反应详情

EQUATION

反应方程式

HRID 17364 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-(4-Bromo-2-cyano-5-fluoro-6-hydroxy-3-methylphenyl)-2,2-dimethyl-3-[(phenylmethyl)oxy]propionamide (I-105) (5.82 g, 13.37 mmol) was dissolved in ethyl acetate (120 ml), carbon-held palladium catalyst (5% wet, 580 mg) was added, followed by vigorously stirring at room temperature under atmospheric pressure of hydrogen for 18 hours. After the reaction, the insoluble matter was separated by filtration through Celite, the filtrate was concentrated under reduced pressure. The resulting residue was recrystallized and purified with n-hexane/ethyl acetate to obtain the entitled compound (2.32 g, 50%) as a white solid.

WORKUP

后处理

  1. additioncarbon-held palladium catalyst (5% wet, 580 mg) was added
  2. customAfter the reaction
  3. customthe insoluble matter was separated by filtration through Celite
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe resulting residue was recrystallized
  6. custompurified with n-hexane/ethyl acetate