HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetoacetate → HCID 89767759, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetoacetate | HCID 8868 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3-Bromo-1,1,1-trifluoro-2-propanone | HCID 79008 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 89767759 | HCID 89767759 | — |
Reaction Steps
To a mixture of ethyl acetoacetate (3.98 mL) in THF (dry) (50 mL) was added NaH (1.571 g) at 0° C., and the mixture was stirred for 30 min at the same temperature. To the mixture was added 3-bromo-1,1,1-trifluoroacetone (5 g) 0° C., and the mixture was stirred for 3 h. The mixture was poured into brine at room temperature and extracted with EtOAc. The organic layer was separated, washed successively with water and brine, dried over MgSO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane) to give the title compound (1.570 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09238639B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-626235c5910f4b0a9b788bcabbf70c27 |
| Source note | uspto-grants-2016_01 |