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

HRID 930552ノート

反応式

HRID 930552 の反応式
[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

参加物

5

反応物 3

HCID 176Acetic Acid2 回HCID 24654Hydrazine hydrate (1:1)2 回HCID 674500244-[4-(Benzylamino)-3-nitrophenyl]-3-methyl-4-oxobutanoic acid

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-43f285e70cfa4190b1449e64e1717aab
出典データセット
uspto-grants-2016_03
特許番号
US09296748B2

反応ノート

読み込み中…