Ethylene Glycol → HCID 57901635, 화합물

HRID 1851521노트

반응식

HRID 1851521 반응식
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[S:6]([NH:9][C:10]1[CH:11]=[CH:12][CH:13]=[C:14]2[C:18]=1[NH:17][C:16]([C:19](=[S:21])[NH2:20])=[CH:15]2)(=[O:8])=[O:7].N[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1S.Cl.C(O)CO>O>[S:21]1[C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=2[N:20]=[C:19]1[C:16]1[NH:17][C:18]2[C:14]([CH:15]=1)=[CH:13][CH:12]=[CH:11][C:10]=2[NH:9][S:6]([C:2]1[S:1][CH:5]=[CH:4][CH:3]=1)(=[O:7])=[O:8]

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 313Hydrochloric AcidHCID 87132-AminothiophenolHCID 57901763HCID 57901763, 화합물

생성물 1

HCID 57901635HCID 57901635, 화합물수율 38%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

A mixture of 7-[(2-thienylsulfonyl)amino]-1H-indole-2-carbothioamide (0.30 g), 2-aminothiophenol (0.10 mL), concentrated hydrochloric acid (0.5 mL) and ethylene glycol (6 mL) was stirred at 100° C. overnight. Water was added to the reaction mixture, and the obtained crystals were filtrated, washed with water and dried. The obtained crystals were subjected to silica gel column chromatography and the title compound (0.14 g, yield 38%) was obtained as colorless crystals from a fraction eluted with ethyl acetate-hexane (2:3, volume ratio). The crystals were recrystallized from ethyl acetate-hexane. melting point 201-202° C.

후처리

  1. filtrationthe obtained crystals were filtrated
  2. washwashed with water
  3. customdried

출처 및 근거

ORD 기록
ord-8c958880148d444dbdd06db112f76a8b
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957070B2

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