HRID1024058
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A mixture of 113h (2 g, 9.05 mmol), 2,6-dibromo-4-fluorobenzyl acetate (101j)(8.8 g, 27.15 mmol), XantPhos (524 mg, 0.9 mmol), Pd2(dba)3 (828 mg, 0.9 mmol) and Cs2CO3 (5.9 g, 18 mmol) in dioxane (200 mL) was heated at 100° C. for 15 h under nitrogen. The reaction mixture was filtered and the filtrated was evaporated in vacuo. The residue was purified by silical-gel column eluting with 1:1 ethyl acetate/petroleum ether to give 113i as a yellow solid (3 g, 71%). MS: (M+H)+ 466.
WORKUP
后处理
- filtrationThe reaction mixture was filtered
- customthe filtrated was evaporated in vacuo
- customThe residue was purified by silical-gel column
- washeluting with 1:1 ethyl acetate/petroleum ether