反应详情

5-({[(4-methoxy-2,6-dimethylphenyl)sulfonyl](methyl)amino}methyl)-2-methylfuran-3-carboxylic acid (82 mg, 0.22 mmol) was dissolved in DCE (1 mL) and CDI (72 mg, 0.33 mmol) was added. The reaction was stirred at ambient temperature for 2 h and 0.5 mL of this solution was added to a flask containing 2-[4-(4,5-dihydro-1H-imidazol-2-yl)phenyl]-N-methylethanamine 0.3 HCl (34 mg, 0.11 mmol) and DIPEA (0.076 mL, 0.44 mmol) in DMF (2 mL). The reaction was stirred at ambient temperature for 3 days, then heated in a microwave at 120° C., 250 psi, 200 W for 2×20 min. The reaction was concentrated and diluted with DCM, then washed with water and saturated brine, and dried over MgSO4. The filtrate was shaken with Ambersep and PL-MIA resins, then filtered. The solvent was removed in vacuo and a portion of the crude product purified using prep method C.

1. stirringThe reaction was stirred at ambient temperature for 3 days
2. temperatureheated in a microwave at 120° C.
3. customfor 2×20 min
4. concentrationThe reaction was concentrated
5. additiondiluted with DCM
6. washwashed with water and saturated brine
7. dry with materialdried over MgSO4
8. stirringThe filtrate was shaken with Ambersep and PL-MIA resins
9. filtrationfiltered
10. customThe solvent was removed in vacuo
11. customa portion of the crude product purified