Methanol → 1,6-Dihydro-5(4H)-pyrimidinone O-(2-propynyl)oxime monohydrochloride
反応式
O.[ClH:2].Cl.[NH2:4][CH2:5][C:6]([CH2:8][NH2:9])=O.Cl.[CH2:11]([O:14][NH2:15])[C:12]#[CH:13].[CH3:16]O>>[ClH:2].[CH2:11]([O:14][N:15]=[C:6]1[CH2:8][NH:9][CH:16]=[N:4][CH2:5]1)[C:12]#[CH:13]参加物
4
実験手順
1,3-diaminoacetone dihydrochloride monohydrate (1.10 g, 6.14 mmol) was dissolved in refluxing methanol and O-(2-propynyl)hydroxylamine hydrochloride (0.730 g, 6.75 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 and heated to reflux. After 24 hours the solvent was removed in vacuo. Crystallization from methanol/ethyl acetate afforded 410 mg (36%) of light-brown material. Mp. 205.0° C.
後処理
- 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
- temperatureheated to reflux
- customAfter 24 hours the solvent was removed in vacuo
- customCrystallization from methanol/ethyl acetate
出典と根拠
- ORDレコード
- ord-98086c9c03a94f4bbefe958470294dc0
- 出典データセット
- uspto-grants-1995_11
- 特許番号
- US05470856
反応ノート
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