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Potassium Acetate → 4-(6-Oxo-1,6-dihydro-pyridazin-3-yloxy)-benzoic acid methyl ester

HRID 215837
ノート
印刷プレビュー

反応式

HRID 215837 の反応式
[CH3:1][O:2][C:3](=[O:18])[C:4]1[CH:9]=[CH:8][C:7]([O:10][C:11]2[N:12]=[N:13][C:14](Cl)=[CH:15][CH:16]=2)=[CH:6][CH:5]=1.C([O-])(=[O:21])C.[K+]>C(O)(=O)C>[CH3:1][O:2][C:3](=[O:18])[C:4]1[CH:9]=[CH:8][C:7]([O:10][C:11]2[CH:16]=[CH:15][C:14](=[O:21])[NH:13][N:12]=2)=[CH:6][CH:5]=1
参加物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 517044Potassium AcetateHCID 606748904-(6-Chloro-pyridazin-3-yloxy)-benzoic acid methyl ester

生成物 1

HCID 672971734-(6-Oxo-1,6-dihydro-pyridazin-3-yloxy)-benzoic acid methyl ester収率 75.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 4-(6-chloro-pyridazin-3-yloxy)-benzoic acid methyl ester (1.0 g, 3.78 mmol) from the previous step and anhydrous potassium acetate (0.526 g, 5.37 mmol) in glacial acetic acid (10 ml) was refluxed for 13 h. The volatiles were evaporated in vacuo and the residue was diluted with dichloromethane (20 ml). The separated solid was collected by filtration, washed with 50% aqueous ethanol (2×5 ml) and water (4×7 ml) and dried to provide 0.7 g (43%) of 4-(6-oxo-1,6-dihydro-pyridazin-3-yloxy)-benzoic acid methyl ester.

後処理

  1. temperaturewas refluxed for 13 h
  2. customThe volatiles were evaporated in vacuo
  3. additionthe residue was diluted with dichloromethane (20 ml)
  4. filtrationThe separated solid was collected by filtration
  5. washwashed with 50% aqueous ethanol (2×5 ml) and water (4×7 ml)
  6. customdried

出典と根拠

ORDレコード
ord-40d6a862e36b40eab8fcda3e1585e20f
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08193192B2

反応ノート

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