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

HRID 399034노트

반응식

HRID 399034 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-81d168ca8998475b8275eb45dc79eac9
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05817691

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