2-Chloroacrylonitrile → 4-Cyano-1-(4-cyanobenzyl)-1H-1,2,3-triazole

HRID 651246

反応式

HRID 651246 の反応式
[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

  1. distillationExcess 2-chloroacrylonitrile is distilled off in vacuo
  2. temperaturethe mixture is cooled to room temperature
  3. customthe precipitated product is isolated by filtration
  4. washwashed with water
  5. customThe product (yield 0.92 g; 88% of theory) of m.p. 93.5-94° C. (recrystallization from ethyl acetate/toluene)
  6. customis obtained
  7. 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

関連ノート

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