Triethylamine → 2-(p-Chlorophenyl)-4-[(3,4-dichlorophenyl)thio]-5-(trifluoromethyl)pyrrole-3-carbonitrile

HRID 399034ノート

反応式

HRID 399034 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([S:9]Cl)[CH:5]=[CH:6][C:7]=1[Cl:8].[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[NH:19][C:20]([C:25]([F:28])([F:27])[F:26])=[CH:21][C:22]=2[C:23]#[N:24])=[CH:14][CH:13]=1.C(N(CC)CC)C>C(Cl)Cl.C(OCC)(=O)C>[Cl:11][C:12]1[CH:13]=[CH:14][C:15]([C:18]2[NH:19][C:20]([C:25]([F:28])([F:26])[F:27])=[C:21]([S:9][C:4]3[CH:5]=[CH:6][C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=3)[C:22]=2[C:23]#[N:24])=[CH:16][CH:17]=1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 110001432-(4-chlorophenyl)-5-(trifluoromethyl)-1H-pyrrole-3-carbonitrileHCID 128785403,4-Dichlorobenzenesulfenyl chloride

生成物 1

HCID 189695992-(p-Chlorophenyl)-4-[(3,4-dichlorophenyl)thio]-5-(trifluoromethyl)pyrrole-3-carbonitrile

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

3,4-Dichlorophenylsulfenyl chloride (1.6 g, 7.49 mmol) is added to a solution of 2-(p-chlorophenyl)-5-trifluoromethylpyrrole-3-carbonitrile (2.02 g, 7.48 mmol) and triethylamine (1.67 g, 16.5 mmol) in methylene chloride. The reaction mixture is stirred at room temperature for 24 hours and concentrated in vacuo to obtain a residue. The residue is slurried in ethyl acetate and the resultant mixture is filtered to remove solids. The filtrate is diluted with hexanes to precipitate a solid which is collected and dried to give the title product as a cream colored solid (mp 94°-97° C.).

後処理

  1. concentrationconcentrated in vacuo
  2. customto obtain a residue
  3. filtrationthe resultant mixture is filtered
  4. customto remove solids
  5. additionThe filtrate is diluted with hexanes
  6. customto precipitate a solid which
  7. customis collected
  8. customdried

出典と根拠

ORDレコード
ord-81d168ca8998475b8275eb45dc79eac9
出典データセット
uspto-grants-1998_10
特許番号
US05817691

反応ノート

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