Potassium Carbonate → 5-Bromo-1H-thieno[3,2-c]pyrazole

온도

95 °C

A mixture of 1-(5-bromo-thieno[3,2-c]pyrazol-1-yl)-ethanone [12.0 g, 49.0 mmol Intermediate (51)], 1,4-dioxane (120 mL), and 2 M aqueous potassium carbonate (80.0 mL) was stirred at 95° C. under nitrogen. After 20 hours, the reaction mixture was cooled to room temperature and then diluted with ethyl acetate (200 mL). The mixture was washed twice with water (100 mL) and brine (100 mL) successively, dried over magnesium sulfate, and concentrated in vacuo. The product was dried under vacuum to give 5-bromo-1H-thieno[3,2-c]pyrazole [9.48 g, 95%, Intermediate (52)] as an off-white solid. TLC Rf 0.26 (silica, 1:1 ethyl acetate/heptane); LC/MS: 202.93 (M+H), RT=2.79 minutes; 1H NMR (300 Mhz, CDCl3) δ 10.8 (br s, 1H), 7.70 (s, 1H), 7.12 (s, 1H).

1. temperaturethe reaction mixture was cooled to room temperature
2. washThe mixture was washed twice with water (100 mL) and brine (100 mL) successively
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe product was dried under vacuum

ORD 기록

ord-8f4ac36f607145f4a1156edd7d657943

출처 데이터셋

uspto-grants-2011_04

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07928231B2