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Methylamine → Tert-butyl 4-{2-[4-cyano-3-(methylamino)phenyl]ethyl}piperazine-1-carboxylate

HRID 1519633
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HRID 1519633 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][N:11]2[CH2:16][CH2:15][N:14]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:13][CH2:12]2)=[CH:5][C:4]=1F)#[N:2].[NH2:25][CH3:26]>CC#N>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][N:11]2[CH2:16][CH2:15][N:14]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:13][CH2:12]2)=[CH:5][C:4]=1[NH:25][CH3:26])#[N:2]
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참가 물질

4

반응물 2

HCID 6329MethylamineHCID 67513450Tert-butyl 4-[2-(4-cyano-3-fluorophenyl)ethyl]piperazine-1-carboxylate

생성물 1

HCID 67517520Tert-butyl 4-{2-[4-cyano-3-(methylamino)phenyl]ethyl}piperazine-1-carboxylate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
120 °C

실험 절차

To a solution of tert-butyl 4-[2-(4-cyano-3-fluorophenyl)ethyl]piperazine-1-carboxylate (100 mg, 0.30 mmol) in CH3CN (10 mL) was added aqueous NH2CH3 (10 mL) in a sealed tube, and then heated to 120° C. overnight. The mixture was extracted with EtOAc, washed with brine, dried over anhydrous sodium sulfate and concentrated. The residue was purified via prep-TLC to afford tert-butyl 4-{2-[4-cyano-3-(methylamino)phenyl]ethyl}piperazine-1-carboxylate.

후처리

  1. extractionThe mixture was extracted with EtOAc
  2. washwashed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified via prep-TLC

출처 및 근거

ORD 기록
ord-37f30f25a7214d07b5e4f1d0f7ebc2c2
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09073882B2

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