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Picolinimidohydrazide → tert-butyl 4-[[(Z)-[amino(pyridin-2-yl)methylidene]amino]carbamoyl]piperidine-1-carboxylate

HRID 1051311
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HRID 1051311 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([OH:16])=O)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(C1NC=CN=1)(C1NC=CN=1)=O.[N:29]1[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=1[C:35](=[N:37][NH2:38])[NH2:36]>ClCCl.O>[NH2:36]/[C:35](/[C:30]1[CH:31]=[CH:32][CH:33]=[CH:34][N:29]=1)=[N:37]\[NH:38][C:14]([CH:11]1[CH2:10][CH2:9][N:8]([C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])[CH2:13][CH2:12]1)=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 70493PicolinimidohydrazideHCID 3928711-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acidHCID 5250894Bis-(1H-imidazol-2-YL)-methanone

생성물 1

HCID 87242610tert-butyl 4-[[(Z)-[amino(pyridin-2-yl)methylidene]amino]carbamoyl]piperidine-1-carboxylate

시약·촉매·용매 2

HCID 962Water용매
HCID 6344
Dichloromethane
용매

실험 절차

To as solution of 1-(tert-butoxycarbonyl) piperidine-4-carboxylic acid 37 g (167 mM) in dichloromethane (300 ml) is added carbonyl diimidazole (1 eq.) in small portion over a period of 30 min. pyridine-2-carbohydrazonamide is then added to reaction mixture and stirred at room temperature for 3 hrs. Dichloromethane is evaporated and reaction mass is then stirred in water for 30 min. solid precipitated is filtered and dried to afford the desired compound.

후처리

  1. additionis then added to reaction mixture
  2. customDichloromethane is evaporated
  3. customreaction mass
  4. customprecipitated
  5. filtrationis filtered
  6. customdried

출처 및 근거

ORD 기록
ord-79d3e14e20cc433e8b425e1a2f85633c
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09387204B2

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