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
- 0 °C
PROCEDURE
实验过程
To a solution of (4-chloro-2-methoxyphenyl)boronic acid (1.0 g, 5.36 mmol) in dichloromethane (5 mL) at 0° C. was added boron tribromide (1 M in dichloromethane, 10 mL, 10 mmol). The reaction was stirred at 0° C. for 1 hour, then allowed to warm to room temperature and stirred as such for 18 hours. The reaction was quenched carefully with water. The resulting precipitate was collected by filtration, to give a white solid, 260 mg. The layers were separated and the organic layer was dried over Na2SO4 and concentrated in vacuo to give a white solid, 300 mg. The two batches of solid were combined to give the title compound as a white solid, 560 mg, in a 61% yield. This material was taken on to Preparation 18 without purification.
WORKUP
后处理
- temperatureto warm to room temperature
- stirringstirred as such for 18 hours
- customThe reaction was quenched carefully with water
- filtrationThe resulting precipitate was collected by filtration
- customto give a white solid, 260 mg
- customThe layers were separated
- dry with materialthe organic layer was dried over Na2SO4
- concentrationconcentrated in vacuo
- customto give a white solid, 300 mg