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p-Toluenesulfonic acid monohydrate → Ethyl 3-acetamido-2-oxo-1,2,3,4-tetrahydroquinoline-3-carboxylate

HRID 2220741
ノート
印刷プレビュー

反応式

HRID 2220741 の反応式
[CH2:1]([O:3][C:4](=[O:23])[C:5]([NH:19][C:20](=[O:22])[CH3:21])([CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[NH2:18])[C:6](OCC)=[O:7])[CH3:2].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CCO>[CH2:1]([O:3][C:4]([C:5]1([NH:19][C:20](=[O:22])[CH3:21])[CH2:11][C:12]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[NH:18][C:6]1=[O:7])=[O:23])[CH3:2]
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 521998p-Toluenesulfonic acid monohydrateHCID 59773563HCID 59773563、化合物

生成物 1

HCID 21853904Ethyl 3-acetamido-2-oxo-1,2,3,4-tetrahydroquinoline-3-carboxylate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 1.0 eq. of 80 and 0.3 eq of p-toluenesulfonic acid hydrate in EtOH was refluxed for 2 hrs. The mixture was then stirred at rt for a time sufficient for reaction completion. After rotary evaporation, 100 mL of saturated aqueous NaHCO3 was added and the mixture was extracted with EtOAc. The combined organic extracts were dried over MgSO4 and vacuum filtered. The filtrate was rotary evaporated and dried under vacuum to yield 81.

後処理

  1. customAfter rotary evaporation, 100 mL of saturated aqueous NaHCO3
  2. additionwas added
  3. extractionthe mixture was extracted with EtOAc
  4. dry with materialThe combined organic extracts were dried over MgSO4 and vacuum
  5. filtrationfiltered
  6. customThe filtrate was rotary evaporated
  7. customdried under vacuum

出典と根拠

ORDレコード
ord-6b6cd9f0470a4ad58c2e29d7b2c89266
出典データセット
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07417152B2

反応ノート

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