HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 49764775, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 49764773 | HCID 49764773 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 49764775 | HCID 49764775 | 57.3% |
Reaction Steps
After dissolving 150 mg of 4-nitro-5-(pentan-2-yl)tetrahydrothiophen-3-ol in 4 ml of dichloromethane, 86 mg of mesyl chloride and 138 mg of triethylamine were gradually dropped thereto at 4° C. The temperature of the solution was allowed to rise to room temperature, and the solution was stirred for 3.5 hours. Water was added to stop the reaction, and the solution was extracted with dichloromethane. The organic layer was dried with magnesium sulfate and concentrated, and then purified by silica gel chromatography (hexane/ethyl acetate=10/1), thereby obtaining 78 mg of 3-nitro-2-(pentan-2-yl)-2,5-dihydrothiophene (yield: 57.3%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08367846B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-e6c2261f79bc42f2ab92be8b0a8247fd |
| Source note | uspto-grants-2013_02 |