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

HRID 473766

반응식

HRID 473766 반응식
[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

참가 물질

8

반응물 5

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

생성물 1

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

시약·촉매·용매 2

HCID 23925Iron촉매HCID 962Water용매3회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-80bd9036820040189b8d57ba2378141e
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637497B2

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