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Hydrochloric Acid → N-[(5-isoquinolyl)sulfonyl]-1,3-cyclohexanediamine

HRID 10597
ノート
印刷プレビュー

反応式

HRID 10597 の反応式
C(OC([NH:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH:11]([NH:15][S:16]([C:19]2[CH:28]=[CH:27][CH:26]=[C:25]3[C:20]=2[CH:21]=[CH:22][N:23]=[CH:24]3)(=[O:18])=[O:17])[CH2:10]1)=O)(C)(C)C.Cl>CO>[CH:24]1[C:25]2[C:20](=[C:19]([S:16]([NH:15][CH:11]3[CH2:12][CH2:13][CH2:14][CH:9]([NH2:8])[CH2:10]3)(=[O:17])=[O:18])[CH:28]=[CH:27][CH:26]=2)[CH:21]=[CH:22][N:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 21979834N-(tert-butoxycarbonyl)-N'-[(5-isoquinolyl)sulfonyl]-1,3-cyclohexanediamine

生成物 1

HCID 21979764N-[(5-isoquinolyl)sulfonyl]-1,3-cyclohexanediamine収率 108.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Intermediate 54 (6 g) obtained above was added to a 10% hydrogen chloride solution in methanol (50 ml) and stirred under reflux by heating for 1.5 hours. The solvent was evaporated under reduced pressure, and the residue was dissolved in a mixed solvent of dichloromethane and ethanol, added with saturated aqueous potassium carbonate and vigorously shaken. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to obtain the title compound (4.9 g).

後処理

  1. temperatureunder reflux
  2. temperatureby heating for 1.5 hours
  3. customThe solvent was evaporated under reduced pressure
  4. dissolutionthe residue was dissolved in a mixed solvent of dichloromethane and ethanol
  5. additionadded with saturated aqueous potassium carbonate
  6. stirringvigorously shaken
  7. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  8. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-3eab5bbdfa2e416eae1d6d8b01877451
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07094789B2

反応ノート

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