HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Ethyl 4,4-difluoroacetoacetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | Ethanamine, 1,1,2,2-tetrafluoro-N,N-dimethyl- | HCID 21945697 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | Ethyl 4,4-difluoroacetoacetate | HCID 67697 | 65.5% |
Reaction Steps
An initial charge of 48 g of ethyl acetate was admixed at RT with a 10% solution of 32.4 g of sodium ethoxide in ethanol. The mixture was stirred at RT for 1 h and then admixed with 36 g of 1,1,2,2-tetrafluoroethyldimethylamine. Subsequently, the solution was stirred at 30° C. for 2 h, admixed with H2O and adjusted to pH 5. After extraction with ethyl acetate and subsequent distillation, 27 g (65%) of ethyl difluoroacetoacetate (boiling point 90-94° C./100 mbar) were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08044231B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-2c4a44d24b614e3ea480352504f6c09c |
| Source note | uspto-grants-2011_10 |