反应详情

温度

65 °C

A mixture of N-[(3S)-1-(7-acetyl-5-chloroquinolin-8-yl)pyrrolidin-3-yl]acetamide (22 mg, 0.066 mmol) and ammonium acetate (51.1 mg, 0.663 mmol) in methanol (0.37 mL) and acetonitrile (0.38 mL) was heated at 65° C. in a sealed tube for 30 minutes. After cooling, sodium cyanoborohydride (8.33 mg, 0.133 mmol) was added to the resultant mixture. The reaction was heated at 65° C. for another 4 hours, then cooled to room temperature, quenched with saturated sodium bicarbonate, and extracted with dichloromethane. The combined extracts were dried over magnesium sulfate and evaporated to dryness (17 mg, 77%). The residue was used directly in the next step. LCMS calculated for C17H22ClN4O(M+H)+: m/z=333.1; found: 333.1.

1. temperatureAfter cooling
2. temperatureThe reaction was heated at 65° C. for another 4 hours
3. temperaturecooled to room temperature
4. customquenched with saturated sodium bicarbonate
5. extractionextracted with dichloromethane
6. dry with materialThe combined extracts were dried over magnesium sulfate
7. customevaporated to dryness (17 mg, 77%)