Hydrazine hydrate (1:1) → N-benzyl-6-hydrazinylpyridine-3-carboxamide

HRID 578937

반응식

HRID 578937 반응식
[CH2:1]([NH:8][C:9](=[O:17])[C:10]1[CH:15]=[CH:14][C:13](Cl)=[N:12][CH:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[NH2:19][NH2:20]>C(O)C>[CH2:1]([NH:8][C:9](=[O:17])[C:10]1[CH:15]=[CH:14][C:13]([NH:19][NH2:20])=[N:12][CH:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 857488N-Benzyl-6-chloro-nicotinamide

생성물 1

HCID 51370238N-benzyl-6-hydrazinylpyridine-3-carboxamide수율 78%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Combined N-benzyl-6-chloronicotinamide (13 g, 52.8 mmol) and ethanol (60 mL) then added hydrazine hydrate (85%, 30 mL) drop wise at room temperature. After the addition, the solution was heated to reflux overnight. The reaction mixture was then concentrated to remove ethanol and a solid was obtained. The solid was collected by filtration, washed with EtOAc (3×20 mL), and dried under reduced pressure to give the title compound (10 g, 78%) as an off-yellow solid.

후처리

  1. customwise at room temperature
  2. additionAfter the addition
  3. temperaturethe solution was heated
  4. temperatureto reflux overnight
  5. concentrationThe reaction mixture was then concentrated
  6. customto remove ethanol
  7. customa solid was obtained
  8. filtrationThe solid was collected by filtration
  9. washwashed with EtOAc (3×20 mL)
  10. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-9e0b4bbe7c7141d8a4a273bca2ec21fb
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040522B2

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