反应详情

温度

60 °C

A mixture of 3.84 g (25.00 mmol) 4-piperdinone hydrochloride and 2.51 g (30.00 mmol) O-methylhydroxylamine hydrochloride in 50 mL of MeOH was stirred for 8 hours at 60° C. and then evaporated down in vacuo. The residue was stirred with saturated aqueous potassium carbonate solution and the aqueous phase was extracted with DCM. The combined organic phases were dried over sodium sulfate, evaporated down in vacuo, and dried. Yield: 2.80 g (87% of theoretical); C6H12N2O (M=128.172); calc.: molpeak (M+H)+: 129; found: molpeak (M+H)+: 129; HPLC-MS: 1.44 minutes (method C).

1. customevaporated down in vacuo
2. stirringThe residue was stirred with saturated aqueous potassium carbonate solution
3. extractionthe aqueous phase was extracted with DCM
4. dry with materialThe combined organic phases were dried over sodium sulfate
5. customevaporated down in vacuo
6. customdried
7. custom1.44 minutes (method C)