HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl benzoate → 1-Phenyl-2-(thiazol-2-yl)ethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl benzoate | HCID 7165 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 2-Methylthiazole | HCID 77129 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-Phenyl-2-(thiazol-2-yl)ethanone | HCID 17887047 | 17% |
Reaction Steps
To a solution of 2-methylthiazole (500 mg, 5.1 mmol) in anhydrous THF (10 mL) at −78° C. under nitrogen was added dropwise n-BuLi (2.5 mol/L, 2.0 mL), after being stirred at this temperature for 1 hour, a solution of ethyl benzoate (1.1 g, 7.3 mmol) in anhydrous THF (5 mL) was added, and the reaction mixture was stirred at room temperature overnight. When TLC (PE:EtOAc=7:1) indicated that the starting materials were consumed, water was added to quench the reaction, and the aqueous layer extracted with EtOAc (10 mL×3). The combined organic layer was washed with brine (10 mL), dried over Na2SO4, filtered, concentrated, and purified by column chromatography (PE:EtOAc=15:1) to afford Intermediate 3 as a yellow oil (170 mg, yield: 17.0%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08741915B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-80d7ee6addf34ef69dbb850eebd5c724 |
| Source note | uspto-grants-2014_06 |