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Hydrazine → 9-Amino-3-ethyl-3H-pyrazolo[4',3':5,6]pyrido[3,4-d]pyridazin-6(7H)-one

HRID 429046
ノート
印刷プレビュー

反応式

HRID 429046 の反応式
[C:1]([C:3]1[C:8]([C:9](OCC)=[O:10])=[CH:7][N:6]=[C:5]2[N:14]([CH2:17][CH3:18])[N:15]=[CH:16][C:4]=12)#[N:2].[NH2:19][NH2:20]>C(O)C>[NH2:2][C:1]1[C:3]2[C:4]3[CH:16]=[N:15][N:14]([CH2:17][CH3:18])[C:5]=3[N:6]=[CH:7][C:8]=2[C:9](=[O:10])[NH:19][N:20]=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 9321HydrazineHCID 867575834-Cyano-1-ethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylic acid, ethyl ester

生成物 1

HCID 183543209-Amino-3-ethyl-3H-pyrazolo[4',3':5,6]pyrido[3,4-d]pyridazin-6(7H)-one収率 60%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

To a suspension of 4-cyano-1-ethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylic acid, ethyl ester (10.0 g, 40.1 mmol) in ethanol (100 mL) was added anhydrous hydrazine (5 eq). This suspension was then heated at 80° C. until starting material was consumed. The reaction was allowed to cool to rt and diluted with water (200 mL). The resulting solid was filtered and washed thoroughly with water until the filtrate was colorless. The solid was dried under vacuum to afford the title compound as a yellow solid (5.5 g, 60%). This material was >90% pure as judged by HPLC and was used directly.

後処理

  1. customwas consumed
  2. temperatureto cool to rt
  3. additiondiluted with water (200 mL)
  4. filtrationThe resulting solid was filtered
  5. washwashed thoroughly with water until the filtrate
  6. customThe solid was dried under vacuum

出典と根拠

ORDレコード
ord-5d62c2453b7c40c59a56c8547fdf3f3a
出典データセット
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06316438B1

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