HRID1164351

反应详情

EQUATION

反应方程式

HRID 1164351 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred and refluxing Grignard-complex, previously prepared starting from 39.7 parts of 1-bromo-4-fluoro-2-methylbenzene and 5.1 parts of magnesium in 225 parts of tetrahydrofuran, are added portionwise 8.4 parts of paraformaldehyde. Upon completion, stirring is continued for 1 hour at reflux. The reaction mixture is cooled and poured onto a mixture of crushed ice and acetic acid. The product is extracted with trichloromethane. The extract is dried, filtered and evaporated. The residue is distilled, yielding 14 parts (47.6%) of 4-fluoro-2-methylbenzenemethanol; bp. 110° C. (water-jet).

WORKUP

后处理

  1. temperaturerefluxing Grignard-complex
  2. custompreviously prepared
  3. stirringUpon completion, stirring
  4. temperatureat reflux
  5. temperatureThe reaction mixture is cooled
  6. extractionThe product is extracted with trichloromethane
  7. customThe extract is dried
  8. filtrationfiltered
  9. customevaporated
  10. distillationThe residue is distilled