Potassium Carbonate → 1-(4-(2-Hydroxyethyl)phenyl)pyrrolidin-2-one

温度

130 °C

A mixture of CuI (0.198 mmol), N,N-dimethylethylamine (0.398 mmol), K2CO3 (3.98 mmol) and pyrrolidin-2-one (3.98 mmol) was purged with nitrogen gas. 2-(4-bromophenyl)ethanol (1.99 mmol) was added and the mixture was purged with purged again with nitrogen. The reaction mixture was stirred at 130° C. overnight. After cooling to room temperature, the reaction mixture was diluted with water (25 mL), NH4OH (5 mL) and the aqueous layer was extracted with dichloromethane (3×40 mL). The combined organic extracts were dried over sodium sulfate and evaporated under reduced pressure; the crude was purified by column chromatography to afford the final product. Yield=37%.

1. customwas purged with nitrogen gas
2. customthe mixture was purged
3. customwith purged again with nitrogen
4. temperatureAfter cooling to room temperature
5. additionthe reaction mixture was diluted with water (25 mL), NH4OH (5 mL)
6. extractionthe aqueous layer was extracted with dichloromethane (3×40 mL)
7. dry with materialThe combined organic extracts were dried over sodium sulfate
8. customevaporated under reduced pressure
9. customthe crude was purified by column chromatography

ORDレコード

ord-cac7aea0fdfc45639101761658c312fb

出典データセット

uspto-grants-2014_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08722720B2