反应详情

(S)-Ethyl 1-((2-amino-2,3-dihydro-1H-inden-5-yl)methyl)-5-(trifluoromethyl)-1H-pyrazole-4-carboxylate (0.102 mmol, 36 mg) was suspended in DCM (2 mL) and DBU (0.306 mmol, 0.046 mL, 46.5 mg) added which caused all solids to go into solution. Propane-2-sulfonyl chloride (0.204 mmol, 0.023 mL, 29.1 mg) was added dropwise and the reaction stirred at room temperature for 1 h. An additional 1 eq of sulfonyl chloride was added and the mixture stirred for a further 3 h before leaving to stand overnight and after this time an additional 2 eq. sulfonyl chloride and 3 eq. DBU added. The mixture was concentrated and purified on reverse phase HPLC to give the desired compound as a clear film (12 mg, 0.026 mmol, 25.6%). 1H NMR (400 MHz, CDCl3) δ 1.36 (m, 9H) 2.85 (m, 2H) 3.15 (m, 1H) 3.30 (m, 2H) 4.20 (m, 1H) 4.31 (m, 3H) 5.49 (s, 1H) 7.02 (m, 2H) 7.20 (d, 1H) 7.99 (s, 1H).

1. stirringthe mixture stirred for a further 3 h
2. custombefore leaving
3. waitto stand overnight
4. concentrationThe mixture was concentrated
5. custompurified on reverse phase HPLC