Triethylamine → 2',2"'-(Dithio)-bis[5'-chloro-4-ethoxy-3-thiophenecarboxanilide]

HRID 614222Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 614222
[CH2:1]([O:3][C:4]1[C:5]([C:9](Cl)=[O:10])=[CH:6][S:7][CH:8]=1)[CH3:2].[Cl:12][C:13]1[CH:14]=[CH:15][C:16]([S:20][S:21][C:22]2[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][C:23]=2[NH2:24])=[C:17]([CH:19]=1)[NH2:18].C(N([CH2:35][CH3:36])CC)C>C(Cl)Cl>[Cl:29][C:26]1[CH:27]=[CH:28][C:22]([S:21][S:20][C:16]2[CH:15]=[CH:14][C:13]([Cl:12])=[CH:19][C:17]=2[NH:18][C:9]([C:5]2[C:4]([O:3][CH2:35][CH3:36])=[CH:8][S:7][CH:6]=2)=[O:10])=[C:23]([CH:25]=1)[NH:24][C:9]([C:5]1[C:4]([O:3][CH2:1][CH3:2])=[CH:8][S:7][CH:6]=1)=[O:10]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 947422,2'-Dithiobis(5-chloroaniline)HCID 125737274-Ethoxy-3-thiophenecarbonyl chloride

Produkt 1

HCID 867363882',2"'-(Dithio)-bis[5'-chloro-4-ethoxy-3-thiophenecarboxanilide]

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A 6.60 g. portion of 4-ethoxy-3-thiophenecarbonyl chloride in 50 ml of methylene chloride is added dropwise to a solution of 5.48 g. of 2,2'-(dithio)bis[5-chloroaniline] and 3.54 g. of triethylamine in 100 ml of methylene chloride as in Example 14. After filtration through magnesium silicate, the filtrate was concentrated to dryness and the residue was recrystallized from methylene chloride:petroleum ether to give 2',2"'-(dithio)-bis[5'-chloro-4-ethoxy-3-thiophenecarboxanilide] as yellow crystals, m.p. 179°-181° C.

Aufarbeitung

  1. filtrationAfter filtration through magnesium silicate
  2. concentrationthe filtrate was concentrated to dryness
  3. customthe residue was recrystallized from methylene chloride

Quellen und Nachweise

ORD-Eintrag
ord-dff199ebefec4b989be18ae78904f4df
Quelldatensatz
uspto-grants-1979_03
Patentnummer
US04144235

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