HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 23000820, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 15462955 | HCID 15462955 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 23000820 | HCID 23000820 | 27% |
Reaction Steps
In a mixed solvent of 15 ml of acetic acid and 10 ml of concentrated hydrochloric acid, 0.44 g (1.1 mmol) of (E)-1-(α-cyclopropylcarbonyl-2-fluorobenzyl)-3-ethoxycarbonylmethylidene-4-mercaptopiperidine were dissolved and the resulting solution was allowed to stand for 12 days at room temperature in a dark place. The reaction mixture was concentrated to dryness, followed by crystallization from ethyl ether. The crystals collected by filtration were purified by chromatography on a silica gel column (eluting solvent: chloroform/methanol=30/1), whereby 0.12 g (yield 27%) of the title compound were obtained as light yellowish white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06087379 |
| Source dataset | uspto-grants-2000_07 |
| ORD ID | ord-1de4e408488a4039880f85c697ace903 |
| Source note | uspto-grants-2000_07 |