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

HRID 973942

反応式

HRID 973942 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.CN(C)[CH:18]=[CH:19][C:20](=[O:26])[CH:21]=[CH:22]N(C)C.Cl>O>[CH3:15][CH:9]1[C:8]([C:5]2[CH:6]=[CH:7][C:2]([N:1]3[CH:22]=[CH:21][C:20](=[O:26])[CH:19]=[CH:18]3)=[CH:3][CH:4]=2)=[N:13][NH:12][C:11](=[O:14])[CH2:10]1

参加物

5

反応物 3

HCID 313Hydrochloric Acid2 回HCID 161928Ici 109,081HCID 534218661,5-Bis(dimethylamino)penta-1,4-dien-3-one

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

実験手順

A mixture of 6-(4-aminophenyl)-5-methyl-4,5-dihydro -3(2H)-pyridazinone (101 mg), 1,5-bis(dimethylamino)-1,4-pentadien-3-one (84 mg) and hydrochloric acid (1N, 0.5 ml) in water (1.5 ml) was stirred at room temperature for 4 hours. More hydrochloric acid (1N, 0.5 ml) was added and the reaction mixture was stirred at room temperature for 18 hours and then under reflux for 4 hours to afford a quantity of red insoluble material. The hot aqueous solvent was decanted off from the insoluble material, was allowed to cool and was seeded to afford the title compound, 41 mg, m.p. 245-249° C.

後処理

  1. stirringthe reaction mixture was stirred at room temperature for 18 hours
  2. temperatureunder reflux for 4 hours
  3. customto afford a quantity of red insoluble material
  4. customThe hot aqueous solvent was decanted off from the insoluble material
  5. temperatureto cool

出典と根拠

ORDレコード
ord-047ece221ab9471f944fd8e0f415ff8a
出典データセット
uspto-grants-1991_11
特許番号
US05066653

関連ノート

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