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Hydrazine hydrate (1:1) → HCID 22380629, 화합물

HRID 895624
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HRID 895624 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[CH2:21][N:22]2C(=O)C3=CC=CC=C3C2=O)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].O.NN>C(O)C>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][CH:11]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[CH2:21][NH2:22])[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 22380593HCID 22380593, 화합물

생성물 1

HCID 22380629HCID 22380629, 화합물수율 74.4%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
40 °C

실험 절차

Subsequently, the resulting crude 1-(tert-butoxycarbonyl)-4-[(2-phthalimidylmethylphenyl)amino]piperidine (420 mg) was dissolved in ethanol (8 ml), added with hydrazine monohydrate (0.23 ml) and stirred at room temperature for 1 hour and at 40° C. for 1 hour. After insoluble matters were removed by filtration from the reaction mixture, the solvent was evaporated under reduced pressure. The residue was added with water (10 ml) and extracted twice with dichloromethane (10 ml). The solvent was evaporated under reduced pressure to obtain 219 mg of 1-(tert-butoxycarbonyl)-4-[(2-aminomethylphenyl)amino]piperidine.

후처리

  1. customAfter insoluble matters were removed by filtration from the reaction mixture
  2. customthe solvent was evaporated under reduced pressure
  3. additionThe residue was added with water (10 ml)
  4. extractionextracted twice with dichloromethane (10 ml)
  5. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-65fe43c19ccb401b87f41623f3dbba7d
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06916822B2

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