HRID1380245

反应详情

EQUATION

反应方程式

HRID 1380245 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 180 parts of ethyl carbonochloridate in 600 parts of trichloromethane was added dropwise a solution of 110 parts of 3-[(4-fluorophenyl)(1-methyl-4-piperidinylidene)methyl]pyridine in 600 parts of trichloromethane. Upon completion, the whole was heated till reflux and stirring at reflux was continued for 16 hours. The reaction mixture was evaporated. The residue was stirred in water and the whole was alkalized with a sodium hydroxide solution. The product was extracted with 4-methyl-2-pentanone. The extract was dried, filtered and evaporated, yielding 100 parts (75%) of ethyl 4-[(4-fluorophenyl)(3-pyridinyl)methylene]-1-piperidinecarboxylate as a residue (intermediate 20).

WORKUP

后处理

  1. temperatureUpon completion, the whole was heated
  2. temperaturetill reflux
  3. temperatureat reflux
  4. customThe reaction mixture was evaporated
  5. stirringThe residue was stirred in water
  6. extractionThe product was extracted with 4-methyl-2-pentanone
  7. customThe extract was dried
  8. filtrationfiltered
  9. customevaporated