Ethanol → Ethyl 4,5-diamino-2-ethoxy-benzoate

HRID 578057ノート

反応式

HRID 578057 の反応式
C([NH:8][C:9]1[C:19]([N+:20]([O-])=O)=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:11]([O:23][CH2:24][CH3:25])[CH:10]=1)C1C=CC=CC=1.C(O)C>[Pd].C1COCC1>[NH2:8][C:9]1[C:19]([NH2:20])=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:11]([O:23][CH2:24][CH3:25])[CH:10]=1

参加物

5

反応物 2

HCID 702EthanolHCID 67233615Ethyl 4-benzylamino-2-ethoxy-5-nitro-benzoate

生成物 1

HCID 67229822Ethyl 4,5-diamino-2-ethoxy-benzoate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

Palladium on charcoal (3.50 g 10%) was added to the product obtained at (655c) (16.7 g, 46.1 mmol) in 200 mL THF with 200 mL ethanol and the mixture was hydrogenated using a Parr apparatur at 60 psi H2 pressure and 50° C. for 3 h. The mixture was filtered, washed with ethanol and the filtrate concentrated i. vac. The residue was triturated with dichloromethane and evaporated to dryness. The product was reacted without further purification.

後処理

  1. customat 60 psi H2 pressure and 50° C.
  2. customfor 3 h
  3. filtrationThe mixture was filtered
  4. washwashed with ethanol
  5. concentrationthe filtrate concentrated i
  6. customThe residue was triturated with dichloromethane
  7. customevaporated to dryness
  8. customThe product was reacted without further purification

出典と根拠

ORDレコード
ord-f2236cc87619431e88883eb50219acde
出典データセット
uspto-grants-2015_05
特許番号
US09040565B2

反応ノート

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