HRID2188238

反应详情

EQUATION

反应方程式

HRID 2188238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 3.74 g of acridan (20 mmol), 69 mg of Pd(OAc)2 (0.3 mmol), 44 mg of tri-t-butylphosphine (0.22 mmol), 2.88 g of sodium t-butoxide (30 mmol), and 6.0 g of 2-(4-bromophenyl)benzothiazole (20 mmol) in 60 mL of toluene was stirred at room temperature for 1 h under inert atmosphere, followed by heating at 50° C. for 1 h. The reaction mixture was cooled to room temperature, filtered and concentrated under reduced pressure. The crude product was purified by column chromatography with 15% ethyl acetate in hexanes. NMR analysis confirmed that 3.1 g of the N-arylated acridan product was isolated.

WORKUP

后处理

  1. temperatureby heating at 50° C. for 1 h
  2. temperatureThe reaction mixture was cooled to room temperature
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe crude product was purified by column chromatography with 15% ethyl acetate in hexanes
  6. customwas isolated