Hydrogen Peroxide → (2-Methylquinolin-4-yl)methanol

HRID 473766

反応式

HRID 473766 の反応式
[CH3:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.S(=O)(=O)(O)O.OO.[OH-:19].[NH4+].[CH3:21]O>O.[Fe]>[CH3:1][C:2]1[CH:11]=[C:10]([CH2:21][OH:19])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1

参加物

8

反応物 5

HCID 784Hydrogen PeroxideHCID 887MethanolHCID 1118Sulfuric AcidHCID 70602-MethylquinolineHCID 14923Ammonium Hydroxide

生成物 1

HCID 10149033(2-Methylquinolin-4-yl)methanol

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 962Water溶媒3 回

実験手順

To a mixture of 2-methylquinoline (43.0 g, 0.3 mol), iron (5.04 g, 0.09 mol), FeSO4.7; H2O (25.0 g, 0.09 mol) in methanol(400 mL) and water (200 mL) was added sulfuric acid (conc., 16.0 mL, 0.3 mol) at 0° C., and then H2O2 (160 mL) was slowly added at 0° C. The mixture was then warmed to room temperature and stirred overnight. The solution was diluted with water, basified with ammonium hydroxide, and extracted with ethyl acetate. The combined extract was washed with brine, dried and concentrated. Recrysatllization from ethyl ether/hexane to give (2-Methylquinolin-4-yl)methanol (12.0 g). ESI (M+H)+ 173.9.

後処理

  1. extractionextracted with ethyl acetate
  2. extractionThe combined extract
  3. washwas washed with brine
  4. customdried
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-80bd9036820040189b8d57ba2378141e
出典データセット
uspto-grants-2014_01
特許番号
US08637497B2

関連ノート

読み込み中…