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

HRID 1710597

반응식

HRID 1710597 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bcdd356ba6e74c68a46abd02d7f4913c
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07790727B2

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