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2-(Ethoxymethylene)propanedinitrile → 5-amino-1-(2,3,4-trichlorophenyl)-1H-pyrazole-4-carbonitrile

HRID 2413084
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HRID 2413084 반응식
[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([Cl:9])[CH:5]=[CH:4][C:3]=1[NH:10][NH2:11].C(O[CH:15]=[C:16]([C:19]#[N:20])[C:17]#[N:18])C>C(OC(O)C)C.O>[NH2:20][C:19]1[N:10]([C:3]2[CH:4]=[CH:5][C:6]([Cl:9])=[C:7]([Cl:8])[C:2]=2[Cl:1])[N:11]=[CH:15][C:16]=1[C:17]#[N:18]
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참가 물질

5

반응물 2

HCID 671522-(Ethoxymethylene)propanedinitrileHCID 129529942,3,4-Trichlorophenylhydrazine

생성물 1

HCID 30189015-amino-1-(2,3,4-trichlorophenyl)-1H-pyrazole-4-carbonitrile수율 52.2%

시약·촉매·용매 2

HCID 962Water용매HCID 101298981-Ethoxyethanol용매

실험 절차

2,3,4-Trichlorophenylhydrazine (21.15 g) and ethoxymethylenemalononitrile (12.8 g) in ethoxyethanol (100 ml) were heated at reflux for one hour. The solution was then cooled and diluted with water. The sticky solid precipitate thus obtained was crystallized from toluene (48 ml) to give 5-amino-4-cyano-1-(2,3,4-trichlorophenyl)pyrazole (15 g), m.p. 154°-156° C., in the form of off-white crystals.

후처리

  1. temperatureat reflux for one hour
  2. temperatureThe solution was then cooled
  3. customThe sticky solid precipitate thus obtained
  4. customwas crystallized from toluene (48 ml)

출처 및 근거

ORD 기록
ord-b5e57a8ee485449bb56c7368f6336246
출처 데이터셋
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04496390

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