HRID2393771

反应详情

EQUATION

反应方程式

HRID 2393771 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

Preparation of 2-trimethylsilyl indole ##STR15## A mixture of iodoaniline (2.19 g, 10 mmol), acyl silane (2.36 g, 20 mmol, prepared according to the procedures of reference example A), DABCO (1,4-diazabicyclo[2.2.2]octane, 3.36 g, 30 mmol) and Pd(OAC)2 (112.25 mg, 0.5 mmol) in 30 mL DMF was degassed via N2 /vacuum and heated at 105° C. for 36 h. The mixture was cooled to room temperature, diluted with IPAc (isopropyl acetate, 100 mL) and washed with 2×50 mL of water. The IPAc layer was concentrated in vacuum and chromatographed over silica gel to give 2-trimethylsilyl indole and indole.

WORKUP

后处理

  1. customprepared
  2. customwas degassed via N2 /vacuum
  3. temperatureThe mixture was cooled to room temperature
  4. additiondiluted with IPAc (isopropyl acetate, 100 mL)
  5. washwashed with 2×50 mL of water
  6. concentrationThe IPAc layer was concentrated in vacuum
  7. customchromatographed over silica gel