HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → (E)-2-(fluoromethylene)-4-(p-fluorophenyl)butan-1-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Ethyl 2-(difluoromethyl)-2-(t-butoxycarbonyl)-4-(p-fluorophenyl)butyrate | HCID 15342051 | — |
| Solvent | Water | HCID 962 | — |
| Product | (E)-2-(fluoromethylene)-4-(p-fluorophenyl)butan-1-ol | HCID 10943450 | — |
Reaction Steps
Add methanesulfonic acid (47.7 kg, 496 mol) to a toluene solution of ethyl 2-(difluoromethyl)-2-(t-butoxycarbonyl)-4-(p-fluorophenyl)butyrate as prepared in Example 3.1 at a temperature of 40° C.-50° C. After 3 to 6 hours, cool the reaction to ambient temperature. Add toluene (91 kg) and water (421 kg) and stir for 30 minutes. Separate the aqueous layer. Add to the organic layer a 20% by weight solution of sodium chloride in water (420 kg) and stir for 30 minutes. Separate the layers to give the title compound as a solution in toluene.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05679854 |
| Source dataset | uspto-grants-1997_10 |
| ORD ID | ord-e2700ddf1f5b487f83cc8bba401518fe |
| Source note | uspto-grants-1997_10 |