HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 13914068, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 23036576 | HCID 23036576 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 13914068 | HCID 13914068 | 69.1% |
Reaction Steps
6.2 g of 2-(3-fluoropropylthio)-1,3-thiazoline-4-one was dissolved in 80 ml of methylene chloride and cooled below 10° C. 5.5 g of methanesulfonyl chloride and 8.9 ml of triethylamine were added dropwise to the solution keeping the temperature below 15° C., followed by stirring at room temperature for 2 hours. After addition of water, the reaction mixture was extracted by methylene chloride, then organic layer is washed with water and dried over anhydrous sodium sulfate, followed by concentration to an oil, which is purified by silica-gel column chromatography to obtain 6.0 g of the objective compound as a pale brown oil (yield: 69.1%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04791127 |
| Source dataset | uspto-grants-1988_12 |
| ORD ID | ord-dd3c8f07c275452abb5bd20c4b1238bf |
| Source note | uspto-grants-1988_12 |