HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3-(1-Benzyloxycarbonyl-4-piperidyl)propyl p-toluenesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| Reactant | Benzyl 4-(3-hydroxypropyl)piperidine-1-carboxylate | HCID 14989193 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | 3-(1-Benzyloxycarbonyl-4-piperidyl)propyl p-toluenesulfonate | HCID 13652731 | 57.8% |
Reaction Steps
To a chilled mixture of 3-(1-benzyloxycarbonyl-4-piperidyl)propanol (110 g) and pyridine (500 ml) is added portionwise tosyl chloride (100 g) for 2 hours with stirring. After stirring for further 1 hour, ice water (1 l) is added dropwise to the mixture. The resulting mixture is acidified by dropwise addition of concentrated hydrochloric acid at ice-bath temperature and extracted with ethyl acetate (1 l). The extract is washed successively with diluted hydrochloric acid and water, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue is crystallized from ethanol to give 3-(1-benzyloxycarbonyl-4-piperidyl)propyl p-toluenesulfonate (99 g) as a colorless crystals, mp 59°-60° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04591458 |
| Source dataset | uspto-grants-1986_05 |
| ORD ID | ord-572987f309a24adea55430a1ae9a1c03 |
| Source note | uspto-grants-1986_05 |