反应详情

3.40 g of 1,4,5,6-tetrahydrocyclopenta[c]pyrazole-3-carbonitrile (CAS-RN 851776-29-9) (25.5 mmol, 1.00 eq) were dissolved in 35 mL dry DMF under nitrogen atmosphere. 7.05 g 2-(bromomethyl)-5-ethoxy-1,3-difluorobenzene (28.1 mmol, 1.10 eq.) and 9.98 g cesiumcarbonate (30.1 mmol, 1.20 eq.) were added and stirred over night at rt. DCM and water were added, the aqueous phase was washed twice with DCM, the organic phase was washed with brine and was dried with magnesiumsulfate, was concentrated in vacuo and purified by flash chromatography (hexane/tert-butyl methyl ether-gradient with hexane 100-70%) to provide 1.07 g (3.45 mmol, 14%) of the analytically pure target compound.

1. washthe aqueous phase was washed twice with DCM
2. washthe organic phase was washed with brine
3. dry with materialwas dried with magnesiumsulfate
4. concentrationwas concentrated in vacuo
5. custompurified by flash chromatography (hexane/tert-butyl methyl ether-gradient with hexane 100-70%)
6. customto provide 1.07 g (3.45 mmol, 14%) of the analytically pure target compound