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Hydrazine hydrate (1:1) → 3-[5-(Benzyloxy)pyridin-2-yl]-1H-pyrazolo[4,3-b]pyridine

HRID 573323
ノート
印刷プレビュー

反応式

HRID 573323 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]([C:17]2[C:22](F)=[CH:21][CH:20]=[CH:19][N:18]=2)=O)=[N:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[NH2:25][NH2:26]>CCO>[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]2[C:17]3=[N:18][CH:19]=[CH:20][CH:21]=[C:22]3[NH:26][N:25]=2)=[N:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 86688982[5-(Benzyloxy)pyridin-2-yl](3-fluoropyridin-2-yl)methanone

生成物 1

HCID 667277533-[5-(Benzyloxy)pyridin-2-yl]-1H-pyrazolo[4,3-b]pyridine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

A mixture of [5-(benzyloxy)pyridin-2-yl] (3-fluoropyridin-2-yl)methanone (2.85 g) and hydrazine monohydrate (1.348 mL) in EtOH (10 mL) was stirred at 50° C. overnight. After cooling, insoluble material was filtrated and washed with EtOH. The filtrate was evaporated, treated with water and extracted with AcOEt. The organic layer was dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (AcOEt/hexane) to give the title compound (0.232 g).

後処理

  1. temperatureAfter cooling
  2. filtrationinsoluble material was filtrated
  3. washwashed with EtOH
  4. customThe filtrate was evaporated
  5. additiontreated with water
  6. extractionextracted with AcOEt
  7. dry with materialThe organic layer was dried over Na2SO4
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (AcOEt/hexane)

出典と根拠

ORDレコード
ord-09bb524c75bb43a7886b07b9575861bf
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09029536B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート