HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen chloride-ethyl acetate → HCID 67399142, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Reactant | HCID 59826886 | HCID 59826886 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67399142 | HCID 67399142 | 69% |
Reaction Steps
To a solution of ethyl 2-cyano-4-(2-fluoropyridin-3-yl)-3-methyl-4-oxobutanoate (19.4 g) in ethyl acetate (20 mL) was added 4 mol/L hydrogen chloride-ethyl acetate solution (90 mL), and the mixture was stirred for 18 hr, and concentrated under reduced pressure. Water was added to the residue, and the mixture was extracted with ethyl acetate. The extract was washed with water, saturated aqueous sodium hydrogen carbonate solution and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate-hexane to give the title compound as yellow crystals (yield 14.3 g, 69%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08933105B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-db73606ff3d94b87980c455da5f7df4b |
| Source note | uspto-grants-2015_01 |