HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → Methyl 5-chloro-2-formylbenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 5-Chloro-2-formylbenzoic acid | HCID 7176209 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Methyl 5-chloro-2-formylbenzoate | HCID 58437623 | 65% |
Reaction Steps
To a heterogeneous mixture of 5-chloro-2-formyl-benzoic acid (1.0 g, 5.42 mmol) and K2CO3 (1.12 g, 8.13 mmol) in DMF (7 ml) was added MeI (0.41 ml, 6.5 mmol) at RT. The reaction mixture was stirred for 4 h then diluted into Et2O and washed with water (2×). The organic layer was dried over Na2SO4, filtered and evaporated to dryness to yield the crude title compound (700 mg, 3.52 mmol, 65%) as a light yellow solid, which was used without further purification. HPLC: AtRet=1.84 min; LC-MS: m/z 199.3 [M+H]+; 1H NMR (400 MHz, DMSO-d6): 3.91 (s, 3H), 7.84-7.94 (m, 3H), 10.33 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09051279B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-4a65d71363bf4d9e95332fd8d83d18cd |
| Source note | uspto-grants-2015_06 |