HRID2185021

反应详情

EQUATION

反应方程式

HRID 2185021 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2-thienylzinc bromide in tetrahydrofuran (0.5M, 5 mL, 2.5 mmol) was added to a solution of N-[3-[2-(diisopropylamino)ethoxy]-4-methoxypheny]-4-iodobenzamide (WO 99/01127) (0.5 g, 1 mmol) in tetrahydrofuran (5 mL) containing tetrakis(triphenylphosphine)palladium(0) (80 mg, 0.06 mmol), and the mixture was stirred at RT for 16 h. The reaction was quenched with saturated ammonium chloride and extracted with ether and dichloromethane. The organic phase was dried (MgSO4), concentrated in vacuo, and chromatographed (silica gel, 5% methanol/dichloromethane) to afford the title compound (0.1 g) MS(ES) m/e 452.8 [M+H]+.

WORKUP

后处理

  1. customThe reaction was quenched with saturated ammonium chloride
  2. extractionextracted with ether and dichloromethane
  3. dry with materialThe organic phase was dried (MgSO4)
  4. concentrationconcentrated in vacuo
  5. customchromatographed (silica gel, 5% methanol/dichloromethane)