反应详情

温度

75 °C

22 mg (0.257 mmol) of O-methylhydroxylamine hydrochloride and 36 μL (0.257 mmol) of triethylamine were added to a solution of 85 mg (0.185 mmol) of 5-[5-(4-chlorophenyl)pyridin-2-ylethynyl]-2-[2-(4-methylpiperidin-1-yl)ethoxy]benzaldehyde (Example 14.1c) in 2 mL of acetonitrile/EtOH (1:1) and the mixture was stirred for 16 hours at 75° C. The reaction mixture was diluted with water and the aqueous phase exhaustively extracted with DCM. The combined organic phases were dried over magnesium sulfate and evaporated down in vacuo. Yield: 40 mg (44% of theoretical); C29H30ClNO3O2 (M=488.020); calc.: molpeak (M+H)+: 488/490 (Cl); found: molpeak (M+H)+: 488/490 (Cl); HPLC-MS: 6.04 minutes (method A).

1. extractionthe aqueous phase exhaustively extracted with DCM
2. dry with materialThe combined organic phases were dried over magnesium sulfate
3. customevaporated down in vacuo
4. custom6.04 minutes (method A)