Ethanol → HCID 136060809、化合物

HRID 1851520ノート

反応式

HRID 1851520 の反応式
[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]

参加物

6

反応物 4

HCID 702EthanolHCID 11858Ethyl 2-chloroacetoacetateHCID 31374DimethylacetamideHCID 57901763HCID 57901763、化合物

生成物 1

HCID 136060809HCID 136060809、化合物収率 73%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-061dd2de1f9e49c1b55500093d200d40
出典データセット
uspto-grants-2015_02
特許番号
US08957070B2

反応ノート

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