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

HRID 5813

반응식

HRID 5813 반응식
[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

참가 물질

5

반응물 3

HCID 313Hydrochloric Acid2회HCID 161928Ici 109,081HCID 534218661,5-Bis(dimethylamino)penta-1,4-dien-3-one

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c82a189b0657442b9a6978acdd19952a
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05246928

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