Hydrogen Bromide → 2-(3-Aminopropyl)-5-bromo-3-methylpyridine

HRID 34928

반응식

HRID 34928 반응식
N[C:2]1[CH:3]=[C:4]([CH3:12])[C:5]([CH2:8][CH2:9][CH2:10][NH2:11])=[N:6][CH:7]=1.N([O-])=O.[Na+].[OH-].[NH4+].[BrH:19]>O.[Cu]>[NH2:11][CH2:10][CH2:9][CH2:8][C:5]1[C:4]([CH3:12])=[CH:3][C:2]([Br:19])=[CH:7][N:6]=1

참가 물질

7

반응물 4

HCID 260Hydrogen BromideHCID 14923Ammonium HydroxideHCID 198517805-Amino-2-(3-aminopropyl)-3-methylpyridineHCID 23668193Sodium Nitrite

생성물 1

HCID 198517812-(3-Aminopropyl)-5-bromo-3-methylpyridine

시약·촉매·용매 2

HCID 23978Copper촉매HCID 962Water용매2회

실험 절차

5-Amino-2-(3-aminopropyl)-3-methylpyridine (8.05 g) in hydrobromic acid (48%, 75 ml) and water (8 ml) wasreacted with cuprous bromide (8.73 g) and copper bronze (0.29 g). A solution of sodium nitrite (5.1 g) in water (8 ml) was added at 5°-8° C. over 40 minutes, the reaction mixture was allowed to stir at 5°-8° C. for one hour and then stirred at room temperature for 3 hours. The cooled reaction mixture was then basified with ammonium hydroxide (70 ml), which was then extracted with chloroform 3×150 ml. The chloroform extracts were then washed with fresh ammonium hydroxide and water (70 ml of each) till no more blue colour was visible in the aqueous layer. Chloroform extracts were dried over magnesium sulphate, filtered and concentrated to dryness to give the title compound (8.2 g) as an amber oil.

후처리

  1. stirringstirred at room temperature for 3 hours
  2. customThe cooled reaction mixture
  3. extractionwas then extracted with chloroform 3×150 ml
  4. washThe chloroform extracts were then washed with fresh ammonium hydroxide and water (70 ml of each) till no more blue colour
  5. dry with materialChloroform extracts were dried over magnesium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-9465c95b41ee425b9b6a12fd598f2ebc
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04764519

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