HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 13518417, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 2,2,2-Trichloroethyl chloroformate | HCID 87063 | — |
| Reactant | 5-Methyl-2h-1,4-thiazin-3(4h)-one | HCID 290017 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 13518417 | HCID 13518417 | 80.7% |
Reaction Steps
2,2,2-Trichloroethylchloroformate (64 ml) was added dropwise to a stirred suspension of 5-methyl-2H-1,4-thiazin-3(4H)-one (50 g) in a mixture of acetonitrile (500 ml)-pyridine (75 ml) under ice-cooling. The mixture was stirred at room temperature for 1 hour and then, poured into cold water (1.5 l) The resulting precipitates were collected by filtration, recrystallized from ethanol to give 5-methyl-6-[1-(2,2,2-trichloroethoxycarbonyl)-1,4-dihydro-4-pyridinyl]-2H-1,4-thiazin-3(4H)-one (120 g, yield 80.7%) as pale yellow prisms.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04804668 |
| Source dataset | uspto-grants-1989_02 |
| ORD ID | ord-813743845e1b4bb19c1eef823a10bade |
| Source note | uspto-grants-1989_02 |