反应详情

温度

100 °C

Into a vessel with condensor, was placed a solution of 4-(1-(3-(2-(2-chloroethyl)-4-methyl-1H-imidazol-5-yl)-4-methylbenzoyl)piperidin-4-yl)benzonitrile (compound 24.1, 26 mg, 0.06 mmol, 1.00 equiv) in EtOH (10 mL). Dimethylamine (1 M in THF, 0.3 mL, 0.3 mmol) was added and the mixture was sealed under a nitrogen balloon. The resulting solution was stirred overnight with a 100° C. oil bath. After cooling to room temperature, the resulting mixture was concentrated under reduced pressure and the crude product was purified by Prep-HPLC with the following conditions (1#-Pre-HPLC-001(SHIMADZU)): Column,) (Bridge Shield RP18 OBD Column, 5 um, 19*150 mm; mobile phase, WATER WITH 0.03% NH3H2O and CH3CN (31% CH3CN up to 43% in 7 min, up to 100% in 0.5 min, down to 31% in 3.5 min); Detector, Waters 2489, 254 & 220 nm. The fractions containing pure compound were combined and lyophilized to yield 6.3 mg (24%) of the title compound as a white solid. m/z (ES+) 456 (M+H)+.

1. customInto a vessel with condensor, was placed
2. customthe mixture was sealed under a nitrogen balloon
3. temperatureAfter cooling to room temperature
4. concentrationthe resulting mixture was concentrated under reduced pressure
5. customthe crude product was purified by Prep-HPLC with the following conditions (1#-Pre-HPLC-001(SHIMADZU))
6. waitmobile phase, WATER WITH 0.03% NH3H2O and CH3CN (31% CH3CN up to 43% in 7 min
7. waitup to 100% in 0.5 min
8. waitdown to 31% in 3.5 min)
9. additionThe fractions containing pure compound