HRID1165408

反应详情

EQUATION

反应方程式

HRID 1165408 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

19.2 g of 2,4-difluoro-3-chloronitrobenzene and 3 g of anhydrous FeCl3 are heated to +140° C., 5.1 ml of bromine are added dropwise with stirring, and the mixture is stirred for a further 48 hours at that temperature. The reaction mixture is cooled and is then taken up in dichloromethane and washed with water. The organic phase is separated off, dried over sodium sulfate and concentrated. The residue is purified on a silica gel column using hexane/dichloromethane (10:1) as eluant. The title compound of formula ##STR10## is obtained in the form of a brown oil; refractive index nD25 : 1.5720.

WORKUP

后处理

  1. stirringthe mixture is stirred for a further 48 hours at that temperature
  2. temperatureThe reaction mixture is cooled
  3. washwashed with water
  4. customThe organic phase is separated off
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe residue is purified on a silica gel column