HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 4,4-Difluoro-3-Methyl-3-Buten-1-Yl Methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 4,4-Difluoro-3-methyl-3-butenol | HCID 15191149 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4,4-Difluoro-3-Methyl-3-Buten-1-Yl Methanesulfonate | HCID 23020237 | 99.9% |
Reaction Steps
To 100 ml of tetrahydrofuran, 4.45 g (36 mmol) of 4,4-difluoro-3-methyl-3-butenol and 4.59 g (40 mmol) of methanesulfonyl chloride were dissolved, followed by drop-wisely adding 4.42 g (44 mmol) of triethylamine under ice-cooling. After the end of the drop-wise addition, the reaction liquid was stirred at room temperature for 1 hour. Hydrochloric acid salt of triethylamine was filtered, followed by adding water to the filtrate and extracting with ethyl acetate. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentrating under reduced pressure to obtain 7.20 g (yield: 99%) of 4,4-difluoro-3-methyl-3-butenyl methanesulfonate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07273878B2 |
| Source dataset | uspto-grants-2007_09 |
| ORD ID | ord-e680c7682ab7466aa6d496a144f3bdf2 |
| Source note | uspto-grants-2007_09 |