Methanol → 1,6-Dihydro-5(4H)-pyrimidinone O-(1-methylethyl)oxime monohydrochloride
반응식
O.[ClH:2].Cl.[NH2:4][CH2:5][C:6]([CH2:8][NH2:9])=O.Cl.[CH3:11][CH:12]([O:14][NH2:15])[CH3:13].[CH3:16]O>>[ClH:2].[CH3:11][CH:12]([O:14][N:15]=[C:6]1[CH2:8][NH:9][CH:16]=[N:4][CH2:5]1)[CH3:13]참가 물질
4
실험 절차
1,3-Diaminoacetone dihydrochloride monohydrate (2.0 g, 11.2 mmol) was dissolved in refluxing methanol and O-(1-methylethyl)hydroxylamine hydrochloride (2.5 g, 22.4 mmol) was added. After refluxing for 48 hours the solvent was evaporated. The crude product was dissolved in methanol and an excess of trimethylorthoformate was added to the reaction mixture which was heated to reflux. After 24 hours the solvent was removed in Vacuo. Crystallization from methanol/ethyl acetate afforded 1.00 g (47%) light-brown material. Mp. 170.0° C.
후처리
- additionwas added
- temperatureAfter refluxing for 48 hours the solvent
- customwas evaporated
- dissolutionThe crude product was dissolved in methanol
- additionan excess of trimethylorthoformate was added to the reaction mixture which
- temperaturewas heated to reflux
- customAfter 24 hours the solvent was removed in Vacuo
- customCrystallization from methanol/ethyl acetate
출처 및 근거
- ORD 기록
- ord-cb0d69c88875414e84b49d71fd746930
- 출처 데이터셋
- uspto-grants-1995_11
- 특허 번호
- US05470856
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