HRID2406378

反应详情

EQUATION

反应方程式

HRID 2406378 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureto warm to room temperature
  2. stirringstirred as such for 18 hours
  3. customThe reaction was quenched carefully with water
  4. filtrationThe resulting precipitate was collected by filtration
  5. customto give a white solid, 260 mg
  6. customThe layers were separated
  7. dry with materialthe organic layer was dried over Na2SO4
  8. concentrationconcentrated in vacuo
  9. customto give a white solid, 300 mg