2-Chloroacrylonitrile → 4-Cyano-1-(4-cyanobenzyl)-1H-1,2,3-triazole
反応式
[C:1]([C:3]1[CH:12]=[CH:11][C:6]([CH2:7][N:8]=[N+:9]=[N-:10])=[CH:5][CH:4]=1)#[N:2].Cl[C:14](=[CH2:17])[C:15]#[N:16]>O>[C:15]([C:14]1[N:10]=[N:9][N:8]([CH2:7][C:6]2[CH:5]=[CH:4][C:3]([C:1]#[N:2])=[CH:12][CH:11]=2)[CH:17]=1)#[N:16]参加物
4
反応条件
- 温度
- 80 °C
実験手順
A mixture of 4-cyanobenzyl azide (0.8 g) and 2-chloroacrylonitrile (0.88 9) in water (5 ml) is stirred at about 80° C. for 20 hours. Excess 2-chloroacrylonitrile is distilled off in vacuo, the mixture is cooled to room temperature and the precipitated product is isolated by filtration and washed with water. The product (yield 0.92 g; 88% of theory) of m.p. 93.5-94° C. (recrystallization from ethyl acetate/toluene) is obtained after drying.
後処理
- distillationExcess 2-chloroacrylonitrile is distilled off in vacuo
- temperaturethe mixture is cooled to room temperature
- customthe precipitated product is isolated by filtration
- washwashed with water
- customThe product (yield 0.92 g; 88% of theory) of m.p. 93.5-94° C. (recrystallization from ethyl acetate/toluene)
- customis obtained
- customafter drying
出典と根拠
- ORDレコード
- ord-5b259ba147ce4c3fa3a12c8236554aa0
- 出典データセット
- uspto-grants-2001_08
- 特許番号
- US06277999B1
反応ノート
読み込み中…