HRID846730

反应详情

EQUATION

反应方程式

HRID 846730 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 12.6 parts of 3-(4-fluoro-2-nitrophenoxy)propanol, 0.9 parts of N,N-dimethylformamide and 150 parts of trichloromethane were added dropwise 8.36 parts of thionyl chloride and stirring was continued for 1 hour at room temperature. The whole was further stirred and refluxed for 3 hours. The reaction mixture was evaporated under methylbenzene. The residue was stirred in petroleumether. The product was filtered off and dried, yielding 7.41 parts (55%) of 1-(3-chloropropoxy)-4-fluoro-2-nitrobenzene; mp. 143.3° C. (intermediate 25).

WORKUP

后处理

  1. stirringThe whole was further stirred
  2. temperaturerefluxed for 3 hours
  3. customThe reaction mixture was evaporated under methylbenzene
  4. stirringThe residue was stirred in petroleumether
  5. filtrationThe product was filtered off
  6. customdried