反应详情

5-(2-Methyl-2H-pyrazol-3-yl)-thiophene-3-carboxylic acid (0.084 g, 0.40 mmol) was dissolved in THF (2 mL) then DIPEA (0.22 mL, 1.3 mmol) and cis-decahydro-quinoline hydrochloride (DHQ [CIS-S]) (0.084 g, 0.48 mmol) were added followed by HATU (0.182 g, 0.48 mmol). The resulting mixture was stirred overnight then the mixture was diluted with water and extracted with DCM (×2). The organics were dried over sodium sulfate, filtered and evaporated. The crude material was purified by chromatography on a silica II cartridge, eluting with 50-100% ethyl acetate in cyclohexane. The fractions containing the desired product were concentrated under vacuum to give the title compound as a colourless oil (0.101 g). LCMS m/z 330.19 [M+H]+ R.T.=10.43 min (Analytical Method 2).

1. extractionextracted with DCM (×2)
2. dry with materialThe organics were dried over sodium sulfate
3. filtrationfiltered
4. customevaporated
5. customThe crude material was purified by chromatography on a silica II cartridge
6. washeluting with 50-100% ethyl acetate in cyclohexane
7. additionThe fractions containing the desired product
8. concentrationwere concentrated under vacuum