Methyl iodide → 2-Bromo-3-methoxy-6-methylpyridine

HRID 1057832노트

반응식

HRID 1057832 반응식
[Br:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[C:4]([CH3:9])[N:3]=1.[C:10](=O)([O-])[O-].[K+].[K+].IC>CC(C)=O>[Br:1][C:2]1[C:7]([O:8][CH3:10])=[CH:6][CH:5]=[C:4]([CH3:9])[N:3]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 119591012-Bromo-6-methylpyridin-3-ol

생성물 1

HCID 109655632-Bromo-3-methoxy-6-methylpyridine수율 88.3%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A stirred mixture of 2-bromo-3-hydroxy-6-methyl-pyridine (7.89 g, 42.0 mmol), potassium carbonate (11.60 g, 83.9 mmol) and iodomethane (8.93 g, 62.9 mmol, 3.92 mL) in acetone (100 mL) was heated under reflux overnight. The mixture was filtered, evaporated and purified on silica gel (hexane:ethyl acetate, 95:5 to 9:1) to give the desired product as a white solid (7.49 g, 88.3%). 1H NMR (500 MHz, CDCl3): δ2.46 (s, 3H), 3.87 (s, 3H), 7.04 (s, 2H).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux overnight
  3. filtrationThe mixture was filtered
  4. customevaporated
  5. custompurified on silica gel (hexane:ethyl acetate, 95:5 to 9:1)

출처 및 근거

ORD 기록
ord-03f7d513ce4340aa899c34ec076c0021
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06515003B1

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