HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl trifluoroacetate → HCID 17967065, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl trifluoroacetate | HCID 9794 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1-(5-(Methylsulfanyl)pyridin-2-yl)ethan-1-one | HCID 20079367 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 17967065 | HCID 17967065 | — |
Reaction Steps
A stirring solution of sodium hydride (0.253 g, 6.31 mmol) in anhydrous tetrahydrofuran (20 mL) was cooled under nitrogen to 0° C. before the addition of 1-(5-methylsulfanyl-pyridin-2-yl)-ethanone (0.880 g, 5.26 mmol) in anhydrous tetrahydrofuran (20 mL). Ethyl trifluoroacetate (0.751 mL, 6.31 mmol) was added dropwise and the reaction allowed to rise in temperature to 22° C., then heated to reflux and stirred under nitrogen for 17 hours. The solvent was removed and the residue partitioned between saturated aqueous ammonium chloride (10 mL) and dichloromethane (10 mL). The aqueous layer was separated and extracted with DCM (×3). The organic layers were combined, dried and the solvent removed to yield the title compound: MS m/z 264 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07235560B2 |
| Source dataset | uspto-grants-2007_06 |
| ORD ID | ord-4778132dfcb84a13844ce6b9088f24dc |
| Source note | uspto-grants-2007_06 |