HRID732467

反应详情

EQUATION

反应方程式

HRID 732467 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

Degas a sealed tube for 5 min and add a suspension 2-benzyloxy-6-chloro-isonicotinic acid methyl ester (1 g, 3.604 mmol), palladium acetate (100 mg, 0.445 mmol), racemic 2,2′-bis-diphenylphosphanyl-[1,1′]binaphthalenyl (307 mg, 0.493 mmol), cesium carbonate (1.2 g, 3.683 mmol) and (R)-sec-butylamine (0.5 mL, 1.387 mmol) in toluene (14 mL). Heat to 105° C. and stir for 20 h. Cool to room temperature, concentrate and purify (silica gel chromatography, eluting with 3:97 ethyl acetate:hexanes) to give the title compound.

WORKUP

后处理

  1. customDegas a sealed tube for 5 min
  2. temperatureCool to room temperature
  3. concentrationconcentrate
  4. custompurify
  5. wash(silica gel chromatography, eluting with 3:97 ethyl acetate:hexanes)