Ethanol → HCID 136060809, 화합물

HRID 1851520노트

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HRID 1851520 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].Cl[CH:23]([C:29](=O)[CH3:30])[C:24]([O:26][CH2:27][CH3:28])=[O:25].C(O)C.CN(C)C(=O)C>O>[CH3:30][C:29]1[N:20]=[C:19]([C:16]2[NH:17][C:18]3[C:14]([CH:15]=2)=[CH:13][CH:12]=[CH:11][C:10]=3[NH:9][S:6]([C:2]2[S:1][CH:5]=[CH:4][CH:3]=2)(=[O:7])=[O:8])[S:21][C:23]=1[C:24]([O:26][CH2:27][CH3:28])=[O:25]

참가 물질

6

반응물 4

HCID 702EthanolHCID 11858Ethyl 2-chloroacetoacetateHCID 31374DimethylacetamideHCID 57901763HCID 57901763, 화합물

생성물 1

HCID 136060809HCID 136060809, 화합물수율 73%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
90 °C

실험 절차

A mixture of 7-[(2-thienylsulfonyl)amino]-1H-indole-2-carbothioamide (0.50 g), ethyl 2-chloro-3-oxobutyrate (0.40 mL), ethanol (4 mL) and N,N-dimethylacetamide (4 mL) was stirred at 90° 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 (0.47 g, yield 73%) was obtained as pale-yellow crystals from a fraction eluted with tetrahydrofuran-hexane (2:1, volume ratio). The crystals were recrystallized from ethyl acetate-hexane. melting point 226-228° C.

후처리

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

출처 및 근거

ORD 기록
ord-061dd2de1f9e49c1b55500093d200d40
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957070B2

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