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

HRID 614222ノート

反応式

HRID 614222 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-dff199ebefec4b989be18ae78904f4df
出典データセット
uspto-grants-1979_03
特許番号
US04144235

反応ノート

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