反应详情

To a solution of (3S)-3-methyl-1-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine (Description 2) (80 mg, 0.259 mmol) in DMF (5 ml) was added 2-methyl-4-pyridinecarboxylic acid (35.6 mg, 0.259 mmol), HOBT.H2O (39.7 mg, 0.259 mmol), HBTU (98 mg, 0.259 mmol) and DIPEA (0.136 ml, 0.778 mmol) and the reaction mixture was stirred at room temperature overnight. DMF was evaporated in vacuo then DCM (5 ml) was added and washed with saturated aq. NaHCO3 solution (5 ml), dried on a phase separation cartridge and evaporated in vacuo. The crude material was dissolved in MeCN/DMSO 1:1 and purified by MDAP. The desired fractions were collected and concentrated in vacuo giving the title compound (74 mg).

1. customDMF was evaporated in vacuo
2. additionDCM (5 ml) was added
3. washwashed with saturated aq. NaHCO3 solution (5 ml)
4. customdried on a phase separation cartridge
5. customevaporated in vacuo
6. dissolutionThe crude material was dissolved in MeCN/DMSO 1:1
7. custompurified by MDAP
8. customThe desired fractions were collected
9. concentrationconcentrated in vacuo