HRID1439769

反应详情

EQUATION

反应方程式

HRID 1439769 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3 ml. of concentrated hydrochloric acid are added, at 0°, to 2.78 g. of 1-chloro-3-(4'-amino-4-biphenylyl)-butan-3-ol [which can be obtained by nitrating 1-chloro-3-(4-biphenylyl)-butan- 3-ol and reducing the resulting 1-chloro-3-(4'-nitro-4-biphenylyl)-butan-3-ol] and a solution of 1.4 g. of NaNO2 in 6 ml. of water is then added at 0°, while stirring. After adding a solution of 0.7 g. of boric acid in 1.5 g. of 60% hydrofluoric acid, the mixture is stirred for 40 minutes and filtered and the product is washed with water, methanol and ether and dried and the resulting diazonium fluoborate is heated to about 150° until decomposition is complete to give 1-chloro-3-(4'-fluoro-4-biphenylyl)-butan-3-ol, m.p. 78° - 79°.

WORKUP

后处理

  1. additionAfter adding a solution of 0.7 g
  2. filtrationfiltered
  3. washthe product is washed with water, methanol and ether
  4. customdried
  5. temperaturethe resulting diazonium fluoborate is heated to about 150° until decomposition