Methylamine → 2,4-Dihydro-5-methoxy-4-methyl-3H-1,2,4-triazol-3-one
反応式
[CH3:1][O:2][C:3](OC)=[N:4][NH:5][C:6]([O:8]C)=O.[CH3:12][NH2:13]>CO>[CH3:1][O:2][C:3]1[N:13]([CH3:12])[C:6](=[O:8])[NH:5][N:4]=1参加物
4
反応条件
- 温度
- 70 °C
実験手順
8.11 g (0.05 mol) of methyl N′-dimethoxymethylenehydrazinecarboxylate were dissolved in 25.4 g of methanol and admixed with 3.26 g (0.105 mol) of methylamine, dissolved in methanol, and the mixture was heated in an autoclave at 70° C. for 14 hours. The reaction mixture was concentrated under reduced pressure and taken up in water (10 ml). The mixture was acidified by addition of conc. HCl. The crystals which precipitated at 4° C. were filtered off and dried. This gave 1.89 g (29.3%) of 5-methoxy-4-methyl-2,4-dihydro-1,2,4-triazol-3-one in the form of a colourless solid. Melting point 146-148° C.
後処理
- concentrationThe reaction mixture was concentrated under reduced pressure
- additionThe mixture was acidified by addition of conc. HCl
- customThe crystals which precipitated at 4° C.
- filtrationwere filtered off
- customdried
出典と根拠
- ORDレコード
- ord-03288de3d1a74ba8ad443b15b9fdc0f6
- 出典データセット
- uspto-grants-2001_06
- 特許番号
- US06248900B1
反応ノート
読み込み中…