HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Chloroethyl chloroformate → 4-(4-Chlorophenyl)tetrahydropyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Chloroethyl chloroformate | HCID 521305 | — |
| Reactant | HCID 18675725 | HCID 18675725 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-(4-Chlorophenyl)tetrahydropyridine | HCID 417378 | 125.4% |
Reaction Steps
To a cold (0° C.) solution of N-benzyl-4-(4-chlorophenyl)-4-methylpiperidine (3) (0.41 g, 1.4 mmol) in CH2Cl2 was 1.1 equivalent of 1-chloroethylchloroformate. The reaction was then heated to reflux for 2 hrs. Excess solvent was removed and the residue was brought up into methanol. The mixture was refluxed for 2 hrs and excess methanol was removed under reduced pressure. Precipitation of the hydrochloride salt 4 by the addition of CH2Cl2 followed by filtration resulted in the quantitative isolation of the desired crystalline product 4 (100%, 0.34 g). MS m/z: (M+210)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653096B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-3e60337677544041ac0ee8b0ea12d91a |
| Source note | uspto-grants-2014_02 |