HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium trimethylsilanolate → 2-(2,3-Difluoro-phenylsulfanyl)-2-methyl-propionic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium trimethylsilanolate | HCID 23668039 | — |
| Reactant | 2-(2,3-Difluoro-phenylsulfanyl)-2-methyl-propionic acid ethyl ester | HCID 59267849 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-(2,3-Difluoro-phenylsulfanyl)-2-methyl-propionic acid | HCID 59267888 | 90.1% |
Reaction Steps
To a solution of 1.64 g (6.31 mmol) of 2-(2,3-difluoro-phenylsulfanyl)-2-methyl-propionic acid ethyl ester in THF (165 mL) at room temperature are added 1.62 g (12.6 mmol) of potassium trimethylsilanolate. The reaction is stirred at room temperature for 18 h. The solvent is removed under reduced pressure and the residue is partitioned between water and diethyl ether. The basic aqueous layer is separated, acidified using 1M aqueous HCl solution to pH 1 and extracted with DCM (3×100 mL). The organic phase is dried over MgSO4, filtered and the filtrate is concentrated under reduced pressure to give 1.32 g of 2-(2,3-difluoro-phenylsulfanyl)-2-methyl-propionic acid as a pale yellow solid. Yield: 90%, ES-MS: m/z 231 [M−H].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08048899B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-21dbe00471564a4a8bb109e47d7a13af |
| Source note | uspto-grants-2011_11 |