2-Hydrazinoethanol → 6-[2-(2-Hydroxyethyl)-5-methyl-3-oxo-2,3,4,5-tetrahydropyridazin-6-yl]-1-methyl-1,2,3,4-tetrahydroquinolin-2-one

HRID 128014

反応式

HRID 128014 の反応式
O=[C:2]([C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]([CH3:19])[C:14](=[O:20])[CH2:13][CH2:12]2)[CH:3]([CH3:8])[CH2:4][C:5]([OH:7])=O.[NH:21]([CH2:23][CH2:24][OH:25])[NH2:22]>C(O)C>[OH:25][CH2:24][CH2:23][N:21]1[C:5](=[O:7])[CH2:4][CH:3]([CH3:8])[C:2]([C:9]2[CH:10]=[C:11]3[C:16](=[CH:17][CH:18]=2)[N:15]([CH3:19])[C:14](=[O:20])[CH2:13][CH2:12]3)=[N:22]1

参加物

4

反応物 2

HCID 80172-HydrazinoethanolHCID 155745774-Oxo-4-(1-methyl-2-oxo-1,2,3,4-tetrahydroquinolin-6-yl)-3-methylbutanoic acid

生成物 1

HCID 234715436-[2-(2-Hydroxyethyl)-5-methyl-3-oxo-2,3,4,5-tetrahydropyridazin-6-yl]-1-methyl-1,2,3,4-tetrahydroquinolin-2-one収率 80.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2.72 g of 4-oxo-4-(1-methyl-2-oxo-1,2,3,4-tetrahydroquinolin-6-yl)-3-methylbutanoic acid and 1.5 g of 2-hydrazinoethanol in 30 ml of ethanol was heated under reflux on a water bath for 2 hours. The reaction mixture was concentrated under reduced pressure and water was added to the residue. The precipitated crystals were filtered off and recrystallized from isopropanol to give 2.5 g of 6-[2-(2-hydroxyethyl)-5-methyl-3-oxo-2,3,4,5-tetrahydropyridazin-6-yl]-1-methyl-1,2,3,4-tetrahydroquinolin-2-one as colorless crystals, melting at 171°-173° C.

後処理

  1. temperatureunder reflux on a water bath for 2 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure and water
  3. additionwas added to the residue
  4. filtrationThe precipitated crystals were filtered off
  5. customrecrystallized from isopropanol

出典と根拠

ORDレコード
ord-7e0bac69001e4998af08aa82ba068df7
出典データセット
uspto-grants-1981_03
特許番号
US04258185

関連ノート

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