反应详情

温度

50 °C

A mixture of the acid 159 (71 mg, 0.115 mmol) and CDI (37 mg, 0.228 mmol) in dry THF (10 mL) was heated at reflux for 2 h under N2. The reaction mixture was cooled 50° C. and a pre-mixed solution of methyl-cyclopropyl sulfonamide (43 mg, 0.349 mmol) and DBU (49 μL, 0.322 mmol) in 2 ml of dry THF was added to the reaction mixture. The reaction was stirred at 50° C. for 18 h. The solvent was evaporated and the residue was dissolved in CHCl3 and washed with citric acid (10% aq). The organic phase was dried with Na2SO4, filtered and the solvent was removed by rotary evaporation. The crude product was purified by HPLC on an Ace-5 C8 column (100×21.2 mm) with a gradient going from 35 to 60% acetonitrile (0.1% TFA) in H2O (0.1% TFA) over 8 minutes. The product was obtained as a white solid (30 mg, 36%), LRMS (M+H) 722.

1. temperaturewas heated
2. temperatureat reflux for 2 h under N2
3. customThe solvent was evaporated
4. dissolutionthe residue was dissolved in CHCl3
5. washwashed with citric acid (10% aq)
6. dry with materialThe organic phase was dried with Na2SO4
7. filtrationfiltered
8. customthe solvent was removed by rotary evaporation
9. customThe crude product was purified by HPLC on an Ace-5 C8 column (100×21.2 mm) with a gradient
10. waitgoing from 35 to 60% acetonitrile (0.1% TFA) in H2O (0.1% TFA) over 8 minutes