反应 #2383773

ord-26ee7c345b06443cb25915c9be1fb57a

反应方程式

BrCc1ccc2ccccc2c1CBr
1,2-bis(bromomethyl)naphthalene
O=C1CCC(=O)N1Br
N-bromosuccinimide
CC(C)(C#N)N=NC(C)(C)C#N
2,2′-azobis(isobutyronitrile)
BrCc1c(C(Br)Br)ccc2ccccc12
1-(bromomethyl)-2-(dibromomethyl)naphthalene
收率 64.0%

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤the reaction mixture was filtered
  2. 2
    洗涤the residue was washed with 150 ml of dichloromethane
  3. 3
    workup.ADDITIONThe combined solution was treated by the column chromatography (silica gel/dichloromethane) without additional treatments and 16 g (the yield: 64%) of a white solid of 1-(bromomethyl)-2-(dibromomethyl)naphthalene
  4. 4
    其他was obtained

实验过程

In 150 ml of carbon tetrachloride, 20 g (64 mmole) of 1,2-bis(bromomethyl)naphthalene and 23 g (130 mmole) of N-bromosuccinimide were suspended. To the obtained suspension, 1.1 g (6.7 mmole) of 2,2′-azobis(isobutyronitrile) was added and the mixture was vigorously stirred at 100° C. for 2 hours. After the reaction was completed, the reaction mixture was filtered and the residue was washed with 150 ml of dichloromethane. The filtrate and the washing were combined. The combined solution was treated by the column chromatography (silica gel/dichloromethane) without additional treatments and 16 g (the yield: 64%) of a white solid of 1-(bromomethyl)-2-(dibromomethyl)naphthalene was obtained.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06489046B1uspto-grants-2002_12