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Hydrazine hydrate (1:1) → HCID 178434176, 화합물

HRID 712504
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HRID 712504 반응식
[C:1]([CH:4]1[C:9](=O)[CH2:8][CH2:7][N:6]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:5]1)(=O)[CH3:2].[NH2:18][NH2:19].O>CCO>[CH3:2][C:1]1[C:4]2[CH2:5][N:6]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:8][C:9]=2[NH:19][N:18]=1
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 53393266tert-Butyl 3-acetyl-4-oxopiperidine-1-carboxylate

생성물 1

HCID 178434176HCID 178434176, 화합물수율 76.5%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
90 °C

실험 절차

To a solution of tert-butyl 3-acetyl-4-oxopiperidine-1-carboxylate (10.00 g, 41.44 mmol, 1.0 eq) in EtOH was added 98% H2NNH2—H2O (3.11 mL, 62.16 mmol, 1.5 eq). The reaction mixture was heated to 90° C. and refluxed for 2.0 h. The resulted mixture was concentrated in vacuo to give two tautomers as yellow oil (7.5 g, 76.5%), and which were used for the next step without further purification. The compound was characterized by the following spectroscopic data: MS (ESI, pos. ion) m/z: 238.31 (M+1);

후처리

  1. temperaturerefluxed for 2.0 h
  2. concentrationThe resulted mixture was concentrated in vacuo

출처 및 근거

ORD 기록
ord-2b80089bd89549628a315f1644c3a0aa
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181277B2

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