Ethanol → HCID 57901597、化合物

HRID 1851430ノート

反応式

HRID 1851430 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].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]

参加物

5

反応物 3

HCID 702EthanolHCID 74852Ethane, 2-bromo-1,1-diethoxy-HCID 57901763HCID 57901763、化合物

生成物 1

HCID 57901597HCID 57901597、化合物収率 9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-fb880798216c411fa1213cfc54325bcb
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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