Ethanol → HCID 57901597, 화합물

HRID 1851430노트

반응식

HRID 1851430 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].Br[CH2:23][CH:24](OCC)OCC.C(O)C>O>[S:21]1[CH:24]=[CH:23][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

5

반응물 3

HCID 702EthanolHCID 74852Ethane, 2-bromo-1,1-diethoxy-HCID 57901763HCID 57901763, 화합물

생성물 1

HCID 57901597HCID 57901597, 화합물수율 9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 7-[(2-thienylsulfonyl)amino]-1H-indole-2-carbothioamide (0.61 g), 1-bromo-2,2-diethoxyethane (0.32 mL) and ethanol (10 mL) was heated under reflux 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 (0.06 g, yield 9%) was obtained as colorless crystals from a fraction eluted with ethyl acetate-hexane (1:1, volume ratio). The crystals were recrystallized from ethyl acetate-hexane. melting point 164-165° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux overnight
  3. filtrationthe obtained crystals were filtrated
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-fb880798216c411fa1213cfc54325bcb
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957070B2

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