反应详情

温度

150 °C

A mixture of 1-(cyclopropylmethyl)-2-neopentyl-5-(piperidin-4-ylmethylsulfonyl)-1H-benzo[d]imidazole (STEP D, 25 mg, 0.062 mmol), 4-chloropyridine hydrochloride (19 mg, 0.12 mmol) and triethylamine (35 microL, 0.25 mmol) in ethanol was stirred at 150° C. under microwave for 3 h. The solvent was removed. The residue was diluted with ethyl acetate and saturated sodium bicarbonate aqueous solution to separate. The aqueous layer was extracted with ethyl acetate (3 mL×2) and the organic layer was filtered through magnesium sulfate column. The filtrate was concentrated in vacuo. The residue was purified by prep-LC-MS (“process A”).

1. customThe solvent was removed
2. additionThe residue was diluted with ethyl acetate and saturated sodium bicarbonate aqueous solution
3. customto separate
4. extractionThe aqueous layer was extracted with ethyl acetate (3 mL×2)
5. filtrationthe organic layer was filtered through magnesium sulfate column
6. concentrationThe filtrate was concentrated in vacuo
7. customThe residue was purified by prep-LC-MS (“process A”)