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4-(cis-3,5-Dimethyl-1-piperazinyl)-2-nitrobenzonitrile → 2-Amino-4-(cis-3,5-dimethyl-1-piperazinyl)benzonitrile

HRID 130416
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반응식

HRID 130416 반응식
[CH3:1][C@H:2]1[NH:7][C@@H:6]([CH3:8])[CH2:5][N:4]([C:9]2[CH:16]=[CH:15][C:12]([C:13]#[N:14])=[C:11]([N+:17]([O-])=O)[CH:10]=2)[CH2:3]1>C(O)C.CO.[Pd]>[NH2:17][C:11]1[CH:10]=[C:9]([N:4]2[CH2:5][C@H:6]([CH3:8])[NH:7][C@H:2]([CH3:1])[CH2:3]2)[CH:16]=[CH:15][C:12]=1[C:13]#[N:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 691981564-(cis-3,5-Dimethyl-1-piperazinyl)-2-nitrobenzonitrile

생성물 1

HCID 590070532-Amino-4-(cis-3,5-dimethyl-1-piperazinyl)benzonitrile

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 887Methanol용매

실험 절차

A solution of the product of Step 1 (186 mg, 0.71 mmol) in ethanol (14 ml) and methanol (3-4 ml) was treated with palladium on charcoal (37 mg, 10% paste) and stirred under an atmosphere of hydrogen for 16 hours. The mixture was then filtered through celite, washing with ethanol and the then evaporated in vacuo. Purification of the residue by mass directed autoprep HPLC gave the title compound (D20) as the formic acid salt. MS (ES+) m/e 231 [M+H]+.

후처리

  1. filtrationThe mixture was then filtered through celite
  2. washwashing with ethanol
  3. customthe then evaporated in vacuo
  4. customPurification of the residue by mass

출처 및 근거

ORD 기록
ord-62f2dbcac9c041e1a1fe36a4b5ded636
출처 데이터셋
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07381728B2

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