HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 13914034, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 23036575 | HCID 23036575 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 13914034 | HCID 13914034 | 78.8% |
Reaction Steps
8 g of 2-isopropylthio-1,3-thiazoline-4-one was dissolved in 100 ml of methylene chloride and cooled below 10° C. Then, 7.8 g of methanesulfonyl chloride and 12.6 ml of triethylamine were added dropwise to the solution below 15° C. with attention to out-break of heat. After that, the reaction was continued with stirring at room temperature for 2 hours. Water was added to the reaction mixture and extracted by ether. The ether layer was washed with water and dried over anhydrous sodium sulfate. The oil obtained by concentration was purified by silica-gel column chromatography to obtain 9.1 g of the objective compound as a pale brown crystal (yield: 78.8%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04791127 |
| Source dataset | uspto-grants-1988_12 |
| ORD ID | ord-f908f3058d70447abe92494a48d5cc43 |
| Source note | uspto-grants-1988_12 |