HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → Methyl 2,3-difluoro-5-nitrobenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 2,3-Difluoro-5-nitrobenzoic acid | HCID 54593790 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Methyl 2,3-difluoro-5-nitrobenzoate | HCID 62662214 | — |
Reaction Steps
Oxalyl chloride (1 ml) and DMF (5 μl) were added to a CH2Cl2 (1.6 ml) solution containing 2,3-difluoro-5-nitrobenzoic acid (1.61 g) obtained in the 1st step, followed by stirring at room temperature for 15 minutes. The reaction solution was poured into a liquid mixture of MeOH/Py (100 ml/1.28 ml) and the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel chromatography (n-hexane:ethyl acetate=1:0 to 4:1). A light yellow solid of methyl 2,3-difluoro-5-nitrobenzoate (1.71 g) was thus obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09051310B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-e96574f100e948fc8f2c384cb915ea24 |
| Source note | uspto-grants-2015_06 |