HRID235188

反应详情

EQUATION

反应方程式

HRID 235188 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To a degassed mixture of 1-(4-methylphenylsulfonyl)-5-bromoindole-3-carboxaldehyde (36.9 g), 1-decyne (16.8 g), in dry triethylamine (200 ml) and dry tetrahydrofuran (150 ml) was added, 1 mole percent of copper (II) iodide and 2 mole percent of bis(triphenylphosphine)palladium (II) chloride. The reaction mixture was stirred at 65° C. for 7 days. The solution was evaporated, and the residue was flash chromatographed (silica gel:4:1, dichloromethane:heptane). The appropriate fractions were collected and evaporated. The residue was recrystallized from hexane to give 23.1 g (50.8%) of product, mp 84°-86° C.

WORKUP

后处理

  1. customThe solution was evaporated
  2. customchromatographed (silica gel:4:1, dichloromethane:heptane)
  3. customThe appropriate fractions were collected
  4. customevaporated
  5. customThe residue was recrystallized from hexane