HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 86670008, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 1-[4-Hydroxy-2-(trifluoromethyl)phenyl]ethan-1-one | HCID 2775108 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86670008 | HCID 86670008 | 98.4% |
Reaction Steps
To a solution of 1-(4-hydroxy-2-trifluoromethyl-phenyl)-ethanone (29.74 g; 145.7 mmol) in CH2Cl2 (300 mL) and THF (120 mL) was added Et3N (24.4 mL; 174.8 mmol), at 0° C. To the resulting mixture was added dropwise a solution of methanesulfonyl chloride (12.5 mL; 160.3 mmol) in CH2Cl2 (60 mL), at 0° C. Subsequently the mixture was stirred overnight at RT, and poured in ice-water. The layers were separated and the organic layer was washed with 1 M aqueous HCl and water; dried (MgSO4), filtered and concentrated in vacuo to afford methanesulfonic acid 4-acetyl-3-trifluoromethyl-phenyl ester (40.47 g), which was used as such.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09227960B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-af1420143ec84ef687589399d3d57657 |
| Source note | uspto-grants-2016_01 |