Methanol → 1,6-Dihydro-5(4H)-pyrimidinone O-methyloxime monohydrochloride
反応式
O.[ClH:2].Cl.[NH2:4][CH2:5][C:6]([CH2:8][NH2:9])=O.[CH3:10][O:11][NH3+:12].[Cl-].[CH3:14]O>>[ClH:2].[CH3:10][O:11][N:12]=[C:6]1[CH2:8][NH:9][CH:14]=[N:4][CH2:5]1参加物
4
実験手順
1,3-Diaminoacetone dihydrochloride monohydrate (2.61 g, 14.6 mmol) was dissolved in refluxing methanol. To this solution o-methylhydroxylamine hydrochloride (2.43 g, 29.2 mmol) was added. After reflexing for 48 hours the solvents were 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 850 mg (36%) of a light-brown crystalline material. Mp. 170.7° C.
後処理
- customthe solvents were 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
出典と根拠
- ORDレコード
- ord-5a0b5e02eefc472db4304a28baf660fa
- 出典データセット
- uspto-grants-1995_11
- 特許番号
- US05470856
反応ノート
読み込み中…