tert-Butyl 4-(2-methoxy-5-nitrophenyl)piperazine-1-carboxylate → Tert-butyl 4-(5-amino-2-methoxyphenyl)piperazine-1-carboxylate

HRID 1710597

反応式

HRID 1710597 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[C:18]([N+:20]([O-])=O)[CH:17]=[CH:16][C:15]=2[O:23][CH3:24])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>CO.[Pd]>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[C:18]([NH2:20])[CH:17]=[CH:16][C:15]=2[O:23][CH3:24])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 1

HCID 18180062tert-Butyl 4-(2-methoxy-5-nitrophenyl)piperazine-1-carboxylate

生成物 1

HCID 10686178Tert-butyl 4-(5-amino-2-methoxyphenyl)piperazine-1-carboxylate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

33 g of 4-(2-Methoxy-5-nitro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (97.8 mmol) were dissolved in 450 mL of methanol. 3 g of 10% Pd/C were added at room temperature under nitrogen atmosphere, and the reaction mixture was hydrogenated for 4 h. The reaction mixture was filtered over Celite, the was solvent evaporated and the remaining residue was treated with 100 mL of diisopropylether. Once crystallization started, the solvent was removed under reduced pressure and the remaining product dried thoroughly. This material was used in subsequent steps without further purification.

後処理

  1. filtrationThe reaction mixture was filtered over Celite
  2. customthe was solvent evaporated
  3. additionthe remaining residue was treated with 100 mL of diisopropylether
  4. customOnce crystallization
  5. customthe solvent was removed under reduced pressure
  6. customthe remaining product dried thoroughly
  7. customThis material was used in subsequent steps without further purification

出典と根拠

ORDレコード
ord-bcdd356ba6e74c68a46abd02d7f4913c
出典データセット
uspto-grants-2010_09
特許番号
US07790727B2

関連ノート

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