HRID1776071
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
A mixture of di-o-tolylamine (Compound 9) (6.00 g, 30.4 mmol), iodobenzene (12.2 g, 60 mmol), Pd(OAc)2 (0.34 g, 1.5 mmol), P(t-Bu)3 (0.6 g, 3 mmol), sodium tert-butoxide (5.76 g, 60 mmol) in toluene (120 mL) was degassed and heated at about 120° C. for 40 hours. The resulting mixture was diluted with ethyl acetate (200 mL), washed with brine, dried over Na2SO4, loaded on silica gel and purified by flash column using eluents of hexanes to give a white solid (Compound 10) (8.2 g, in 98% yield).
WORKUP
后处理
- customwas degassed
- additionThe resulting mixture was diluted with ethyl acetate (200 mL)
- washwashed with brine
- dry with materialdried over Na2SO4
- custompurified by flash column