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

HRID 578937

反応式

HRID 578937 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 51370238N-benzyl-6-hydrazinylpyridine-3-carboxamide収率 78%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9e0b4bbe7c7141d8a4a273bca2ec21fb
出典データセット
uspto-grants-2015_05
特許番号
US09040522B2

関連ノート

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