1-Chloromethyl-1H-1,2,4-triazole → Diethyl [(1H-1,2,4-triazol-1-yl)methyl]phosphonate
反応式
Cl[CH2:2][N:3]1[CH:7]=[N:6][CH:5]=[N:4]1.[P:8]([O-:15])([O:12][CH2:13][CH3:14])[O:9][CH2:10][CH3:11].[Na+]>C(#N)C>[N:3]1([CH2:2][P:8](=[O:15])([O:12][CH2:13][CH3:14])[O:9][CH2:10][CH3:11])[CH:7]=[N:6][CH:5]=[N:4]1参加物
4
実験手順
A mixture of 18.2 g (0.155 mole) of 1-chloromethyl-1H-1,2,4-triazole, 27.2 g (0.17 mole) of sodium diethyl phosphite and 200 ml of acetonitrile is heated for 2 hours to 60° C. and then refluxed for 16 hours. The precipitate is removed and the solution is concentrated. Fractional distillation of the residue yields 19.1 g (56.5%) of diethyl (1H-1,2,4-triazol-1-yl)methylphosphonate in the form of a colourless oil with a boiling point of 120°-129° C./0.053 mb.
後処理
- temperatureis heated for 2 hours to 60° C.
- temperaturerefluxed for 16 hours
- customThe precipitate is removed
- concentrationthe solution is concentrated
- distillationFractional distillation of the residue
出典と根拠
- ORDレコード
- ord-3c08085d75ff4063baf47e8fb5a554e8
- 出典データセット
- uspto-grants-1985_02
- 特許番号
- US04497647
反応ノート
読み込み中…