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Ethanol → HCID 59314223、化合物

HRID 1047916
ノート
印刷プレビュー

反応式

HRID 1047916 の反応式
[CH2:1]([O:3][C:4]([C:6]1([C:15](=[O:27])[NH:16][C:17]2[CH:26]=[CH:25][CH:24]=[C:23]3[C:18]=2[CH:19]=[CH:20][N:21]=[CH:22]3)[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1)=[O:5])[CH3:2].CCO>[Pt](=O)=O.C(O)(=O)C>[CH2:1]([O:3][C:4]([C:6]1([C:15](=[O:27])[NH:16][C:17]2[CH:26]=[CH:25][CH:24]=[C:23]3[C:18]=2[CH2:19][CH2:20][NH:21][CH2:22]3)[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1)=[O:5])[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

5

反応物 2

HCID 702EthanolHCID 59314243HCID 59314243、化合物

生成物 1

HCID 59314223HCID 59314223、化合物収率 99%

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 176Acetic Acid溶媒

実験手順

A 100 mL Parr reaction vessel is charged with 2-(Isoquinolin-5-ylcarbamoyl)-indan-2-carboxylic acid ethyl ester (320, 500 mg, 1.39 mmol) and EtOH (10 mL). The reaction vessel is agitated by swirling until dissolution ° C. curred. Acetic acid (10 mL) and platinum (IV) oxide (117 mg, 0.52 mmol) are added. The vessel is fitted on a Parr hydrogenation apparatus, flushed with N2 and then evacuated. The vessel is charged with hydrogen to 50 psi. The apparatus is set to agitate. After 4 h, agitation is ceased. The reaction vessel is evacuated and flushed with nitrogen. This process is repeated. The contents of the reaction vessel are diluted with iPrOH (50 mL) and filtered through a pad of celite. Solvent is removed from the filtrate under reduced pressure. The resulting residue is reconstituted in iPrOH (15 mL) and toluene (15 mL). The solvent is removed under reduced pressure. This process is repeated. Pumping to constant weight yields light beige solid (0.5 g, 99%).

後処理

  1. customA 100 mL Parr reaction vessel
  2. dissolutionby swirling until dissolution ° C
  3. customThe vessel is fitted on a Parr hydrogenation apparatus
  4. customflushed with N2
  5. customevacuated
  6. additionThe vessel is charged with hydrogen to 50 psi
  7. stirringto agitate
  8. customThe reaction vessel is evacuated
  9. customflushed with nitrogen
  10. additionThe contents of the reaction vessel are diluted with iPrOH (50 mL)
  11. filtrationfiltered through a pad of celite
  12. customSolvent is removed from the filtrate under reduced pressure
  13. customThe solvent is removed under reduced pressure

出典と根拠

ORDレコード
ord-03cd3320d718463899a00bc0e72f1aae
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08569535B2

反応ノート

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