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

HRID 614222노트

반응식

HRID 614222 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-dff199ebefec4b989be18ae78904f4df
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04144235

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