HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → Methyl 4,4'-difluorobenzilate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | Bis(4-fluorophenyl)(hydroxy)acetic acid | HCID 12068839 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | Methyl 4,4'-difluorobenzilate | HCID 12068840 | — |
Reaction Steps
25.0 g (0.095 mol) of 4,4′-difluorobenzilic acid are added to freshly prepared sodium ethoxide solution containing 2.17 g (0.095 mol) of sodium and 200 mL of ethanol at 20° C. and stirred for 3 h. The solution is evaporated to dryness, the residue is dissolved in DMF, 22.57 g (0.16 mol) of methyl iodide are added dropwise at 20° C. and the mixture is stirred for 24 h. It is worked up and purified analogously to compound 3b. Yield: 21.06 g of 11 (80% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07569581B2 |
| Source dataset | uspto-grants-2009_08 |
| ORD ID | ord-3503d900892f41eba752f339466c8174 |
| Source note | uspto-grants-2009_08 |