HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexane → Methyl 2,3-difluoro-4-methylbenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Trimethylsilyldiazomethane | HCID 167693 | — |
| Reactant | 2,3-Difluoro-4-methylbenzoic acid | HCID 2774141 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methyl 2,3-difluoro-4-methylbenzoate | HCID 55255640 | 100% |
Reaction Steps
To a solution of 2,3-difluoro-4-methyl-benzoic acid (5.0 g, 29 mmol) in CH2Cl2 (20 mL) and MeOH (20 mL) is added 2.0 M TMSCHN2 in hexane (17.5 mL, 34.9 mmol) at 0° C. The reaction mixture is stirred for 1.0 h. The reaction mixture is concentrated to a residue and the residue is purified by flash chromatography to afford the title compound as an oil (5.7 g, 100%). LC-ES/MS m/e 208.3 (M+23).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07846960B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-c012a4255c2d486789dcc7a48d8d1ec1 |
| Source note | uspto-grants-2010_12 |