HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → Methyl 2-fluoro-3-methylbenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | 2-Fluoro-3-methylbenzoic acid | HCID 2737379 | — |
| Product | Methyl 2-fluoro-3-methylbenzoate | HCID 22049929 | 100% |
Reaction Steps
To a solution of 2-fluoro-3-methylbenzoic acid (12.4 g, 80.2 mmol) in methanol (100 mL) at 0° C. was added thionyl chloride (14 g, 120.3 mmol) dropwise. The reaction mixture was stirred at reflux until complete by TLC (1-2 h). After cooling to room temperature, the mixture was partitioned between sat. NaHCO3 and ethyl acetate. The combined organic layers were dried (Na2SO4), filtered and concentrated to give methyl 2-fluoro-3-methylbenzoate as a yellow oil (13.8 g, 100%): 1H NMR (300 MHz, CDCl3) δ 7.74 (t, J=8.1 Hz, 1H), 7.37 (t, J=7.8 Hz, 1H), 7.08 (t, J=7.5 Hz, 1H), 3.90 (s, 3H), 2.31 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09045501B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-0bf081f570c64b919e702333e44f3973 |
| Source note | uspto-grants-2015_06 |