HRID1858085

反应详情

EQUATION

反应方程式

HRID 1858085 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a suspension of 4-chloro-2-[2-(3,5-dimethylphenyl)-acetylamino]-5-iodo-benzoic acid methyl ester (2.39 g in 12 mL N,N-dimethylformamide) and 0.183 g bis(triphenylphosphine)palladium(II) chloride was added 2.02 mL allyltin and the mixture heated to 100° C. on an oil bath. After 2 hours, the mixture was cooled, partitioned between ethyl acetate and water and the organic layer washed further with brine. Concentration of the dried (magnesium sulfate) organics and purification by flash chromatography on silica gel (hexane:ethyl acetate, 95:5; then 90:10) gave the title compound (1.4 g).

WORKUP

后处理

  1. temperaturethe mixture was cooled
  2. custompartitioned between ethyl acetate and water
  3. washthe organic layer washed further with brine
  4. dry with materialConcentration of the dried (magnesium sulfate) organics
  5. custompurification by flash chromatography on silica gel (hexane