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

HRID 973929

반응식

HRID 973929 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.O1[CH:21]=[CH:20][C:19](=[O:22])[CH:18]=[CH:17]1.Cl.N>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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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 recrystallised 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.).

후처리

  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. customThe product was recrystallised first from water to which a little 2N NaOH
  5. additionwas added

출처 및 근거

ORD 기록
ord-b30ff61ef01d49c3a4b11f3734072464
출처 데이터셋
uspto-grants-1991_11
특허 번호
US05066653

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