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Ammonia → HCID 13561854、化合物

HRID 979405
ノート
印刷プレビュー

反応式

HRID 979405 の反応式
[C:1](Cl)(=[O:4])[CH2:2][CH3:3].[NH2:6][C:7]1[N:11]([C:12]2[CH:17]=[CH:16][C:15]([O:18][C:19]([F:22])([F:21])[F:20])=[CH:14][C:13]=2[Cl:23])[N:10]=[CH:9][C:8]=1[C:24]#[N:25].N1C=CC=CC=1.N>C(Cl)(Cl)Cl.C(O)C>[C:24]([C:8]1[CH:9]=[N:10][N:11]([C:12]2[CH:17]=[CH:16][C:15]([O:18][C:19]([F:21])([F:22])[F:20])=[CH:14][C:13]=2[Cl:23])[C:7]=1[NH:6][C:1](=[O:4])[CH2:2][CH3:3])#[N:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 222AmmoniaHCID 1049PyridineHCID 62324Propionyl chlorideHCID 135618335-Amino-4-cyano-1-(2-chloro-4-trifluoromethoxy-phenyl)-pyrazole

生成物 1

HCID 13561854HCID 13561854、化合物収率 75.3%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 6212
Chloroform
溶媒
2 回

実験手順

10 ml (0.11 mole) of propionyl chloride are added to 2.9 g (0.01 mole) of 5-amino-4-cyano-1-(2-chloro-4-trifluoromethoxy-phenyl)-pyrazole in 30 ml of chloroform at 0° C., with stirring, and a solution of 1.8 ml (0.02 mole) of pyridine in 15 ml of chloroform is then added, also at 0° C. When the addition has ended, stirring is continued at room temperature for 20 hours, the solvent is stripped off, the residue is taken up in 50 ml of ethanol, aqueous ammonia is added until the reaction is alkaline, the volatile constituents are removed in vacuo, the residue is taken up in 100 ml of chloroform, the mixture is washed with water, then with 2N aqueous hydrochloric acid and again with water and dried over sodium sulphate and the solvent is removed in vacuo. 2.7 g (75.3% of theory) of 4-cyano-1-(2-chloro-4-trifluoromethoxy-phenyl)-5-propionylamino-pyrazole of melting point 127° C. are obtained.

後処理

  1. additionWhen the addition
  2. stirringstirring
  3. customthe volatile constituents are removed in vacuo
  4. washthe mixture is washed with water
  5. dry with materialwith 2N aqueous hydrochloric acid and again with water and dried over sodium sulphate
  6. customthe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-9609ae51f0e64e44a62bf13633202487
出典データセット
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04668280

反応ノート

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