Ammonia → 4,5-Dihydro-5-methyl-6-(4-(4-oxo-1(4H)-pyridinyl)phenyl)-3(2H)-pyridazinone

HRID 1164801

反応式

HRID 1164801 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]([CH3:15])[CH2:10][C:11](=[O:14])[NH:12][N:13]=2)=[CH:4][CH:3]=1.O1[CH:21]=[CH:20][C:19](=[O:22])[CH:18]=[CH:17]1.Cl.N.[OH-].[Na+]>O>[CH3:15][CH:9]1[C:8]([C:5]2[CH:6]=[CH:7][C:2]([N:1]3[CH:21]=[CH:20][C:19](=[O:22])[CH:18]=[CH:17]3)=[CH:3][CH:4]=2)=[N:13][NH:12][C:11](=[O:14])[CH2:10]1

参加物

7

反応物 5

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 79684H-pyran-4-oneHCID 14798Sodium HydroxideHCID 161928Ici 109,081

生成物 1

HCID 1307024,5-Dihydro-5-methyl-6-(4-(4-oxo-1(4H)-pyridinyl)phenyl)-3(2H)-pyridazinone

試薬・触媒・溶媒 1

HCID 962Water溶媒4 回

実験手順

A stirred mixture of 6-(4-aminophenyl)-5-methyl-4,5-dihydro-3(2H)-pyridazinone (1.0 g), 4H-pyran-4-one (0.52 g), water (20 ml), and concentrated hydrochloric acid (0.41 ml) was heated under reflux for 31/2 hours. The resultant solid was dissolved in the minimum of hot water and the solution was neutralised with aqueous ammonia to give the crude product, 1.16 g, m.p. 249°-256° C. The product was recyrstallised first from water to which a little 2N NaOH was added, and then from water alone to give the pure title compound, 0.82 g, m.p. 254°-256° C. (after melting and resolidifying at about 150° C.).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 31/2 hours
  3. customto give the crude product, 1.16 g, m.p. 249°-256° C
  4. additionwas added

出典と根拠

ORDレコード
ord-f04b32dbc4b34b80b4d17bed1319ee96
出典データセット
uspto-grants-1990_03
特許番号
US04906628

関連ノート

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