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Formic Acid → HCID 19786355、化合物

HRID 1656891
ノート
印刷プレビュー

反応式

HRID 1656891 の反応式
[NH2:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([O:13][C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[CH:4][C:3]=1[C:19]#N.C(O)=[O:22]>[Ni]>[NH2:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([O:13][C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[CH:4][C:3]=1[CH:19]=[O:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 284Formic AcidHCID 135618335-Amino-4-cyano-1-(2-chloro-4-trifluoromethoxy-phenyl)-pyrazole

生成物 1

HCID 19786355HCID 19786355、化合物収率 62%

試薬・触媒・溶媒 1

HCID 935Nickel触媒

実験手順

12 g (0.042 mol) of 5-amino-4-cyano-1-(2-chloro-4-trifluoromethoxy-phenyl)-pyrazole are boiled under reflux with 5 g of Raney nickel in 50 ml of 75% strength aqueous formic acid for 1 hour; the still warm solution is filtered under suction, the residue is rinsed with water, the filtrate is extracted several times with ether, and the combined ether phases are washed with saturated sodium bicarbonate solution, dried over sodium sulphate and evaporated down in vacuo. 8.0 g (62% of theory) of 5-amino-1-(2-chloro-4-trifluoromethoxy-phenyl)-4-formylpyrazole are obtained in the form of an oil.

後処理

  1. filtrationthe still warm solution is filtered under suction
  2. washthe residue is rinsed with water
  3. extractionthe filtrate is extracted several times with ether
  4. washthe combined ether phases are washed with saturated sodium bicarbonate solution
  5. dry with materialdried over sodium sulphate
  6. customevaporated down in vacuo

出典と根拠

ORDレコード
ord-26cf8a5d8b93474dab56a66f3dfca75b
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05256634

反応ノート

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