Acetic Acid → 6-(4-benzylamino-3-nitrophenyl)-5-methyl-4,5-dihydro-2H-pyridazin-3-one

HRID 930552노트

반응식

HRID 930552 반응식
[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([C:15](=O)[CH:16]([CH3:21])[CH2:17][C:18](O)=[O:19])=[CH:11][C:10]=1[N+:23]([O-:25])=[O:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.[NH2:27][NH2:28].C(O)(=O)C>C(O)C>[CH2:1]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:16]([CH3:21])[CH2:17][C:18](=[O:19])[NH:27][N:28]=2)=[CH:11][C:10]=1[N+:23]([O-:25])=[O:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 176Acetic Acid2회HCID 24654Hydrazine hydrate (1:1)2회HCID 674500244-[4-(Benzylamino)-3-nitrophenyl]-3-methyl-4-oxobutanoic acid

생성물 1

HCID 117246806-(4-benzylamino-3-nitrophenyl)-5-methyl-4,5-dihydro-2H-pyridazin-3-one

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
100 °C

실험 절차

4-(4-Benzylamino-3-nitro-phenyl)-3-methyl-4-oxo-butyric acid E-4.1″ (939 mg; 2.74 mmol) is placed in 7 ml ethanol and treated with hydrazine hydrate (0.16 ml; 3.29 mmol) and acetic acid (78.58 μl; 1.37 mmol). The reaction mixture is heated up to 100° C. for 2 hours. Another portion of hydrazine hydrate (0.08 ml; 1.65 mmol) and 40 μl acetic acid are added and stirred for 2 hours at 100° C. After letting the reaction cooling to RT, the product precipitates. It is filtered off and washed with methanol and dried under reduced pressure.

후처리

  1. temperaturecooling to RT
  2. customthe product precipitates
  3. filtrationIt is filtered off
  4. washwashed with methanol
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-43f285e70cfa4190b1449e64e1717aab
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09296748B2

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