Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Methylhydrazine | HCID 6061 | — |
| Reactant | Butanoic acid, 4,4-difluoro-3-oxo-, ethyl ester | HCID 67697 | — |
| Solvent | tert-Butyl methyl ether | HCID 15413 | — |
| Product | HCID 178481857 | HCID 178481857 | 99.9% |
Reaction Steps
166 g (1 mol) of ethyl 4,4-difluoro-3-oxobutanoate were charged in 500 ml of methyl tert-butyl ether and treated with 140 g of formic acid. After cooling of the mixture to 5° C., 119 g (as 40% aqueous solution) of monomethylhydrazine were added. The mixture was then stirred for 20 h at 22° C. The phases were separated, and the organic phase was washed with 200 ml of water and dried over MgSO4. After the removal of the solvent under reduced pressure, 148 g of the product was obtained as an yellow solid having an m.p. of 133° C. and a purity of 95%. Yield 95%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09145369B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-7625eac0e79144fa8234a02130d7736d |
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| Source note | uspto-grants-2015_09 |
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