HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thiazole → HCID 70393644, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thiazole | HCID 9256 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | 5-Methyl-2h-1,4-thiazin-3(4h)-one | HCID 290017 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 70393644 | HCID 70393644 | 23.8% |
Reaction Steps
Ethylchloroformate (3.6 g) was added dropwise to a solution of thiazole (5.7 g) in dichloromethane (72 ml) under ice-cooling, and the mixture was stirred for 30 minutes. Then, 5-methyl-2H-1,4-thiazin-3(4H)-one (3.6 g) was added dropwise to the mixture. The reaction mixture was further stirred at ambient temperature for 5 hours. The mixture was washed with 2N hydrochloric acid and successively with water, was dried over anhydrous magnesium sulfate and the solvent was removed. The residue was chromatographed on silica gel (Wakogel C-200) column, using ethyl acetate-n-hexane (=1:1) as an eluant and was recrystallized from ethanol to give the titled compound (1.9 g, yield 23.8%) as white needles.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04800201 |
| Source dataset | uspto-grants-1989_01 |
| ORD ID | ord-86fda96fee3247b3a124763ed371c48e |
| Source note | uspto-grants-1989_01 |