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

HRID 651246

반응식

HRID 651246 반응식
[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]

참가 물질

4

반응물 2

HCID 701982-ChloroacrylonitrileHCID 110736914-(Azidomethyl)benzonitrile

생성물 1

HCID 217118034-Cyano-1-(4-cyanobenzyl)-1H-1,2,3-triazole

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5b259ba147ce4c3fa3a12c8236554aa0
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06277999B1

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