HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroformate → Ethyl 4-[(4-fluorophenyl)(3-pyridinyl)methylene]-1-piperidinecarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | 3-[(4-Fluorophenyl)(1-methyl-4-piperidinylidene)methyl]pyridine | HCID 13520016 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | Ethyl 4-[(4-fluorophenyl)(3-pyridinyl)methylene]-1-piperidinecarboxylate | HCID 23326079 | 75% |
Reaction Steps
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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04581171 |
| Source dataset | uspto-grants-1986_04 |
| ORD ID | ord-7ac9c2d2b74c4e9fa8b95baac880f409 |
| Source note | uspto-grants-1986_04 |