反应详情

温度

50 °C

Add 2-bromo-4-methanesulfonyl-thiophene (241 mg, 1.0 mmol), caesium fluoride ( 304 mg, 2.0 mmol) and tetrakis-(triphenylphosphin)-palladium(0) (58 mg, 0.05 mmol) to a solution of 3-cyclopentyl-2-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-prop-2-en-1-ol (252 mg, 1.0 mmol) in THF. Stir at 50° C. for 24 h, monitore completion of the reaction by LCMS. Treat the reaction mixture with water and extract with ethyl acetate. Dry organic layers over sodium sulfate and remove solvents under vacuum to obtain 405 mg crude product. Purify by silica gel chromatography, eluting with gradient from 9:1 to 1:1 hexane:ethyl acetate to obtain 118 mg purified product. MS (m/e): 309.0 (M+Na).

1. custommonitore completion of the reaction by LCMS
2. extractionextract with ethyl acetate
3. customDry organic layers over sodium sulfate and remove solvents under vacuum
4. customto obtain 405 mg crude product
5. customPurify by silica gel chromatography
6. washeluting with gradient from 9:1 to 1:1 hexane
7. customethyl acetate to obtain 118 mg
8. custompurified product