Sodium Hydroxide → 3,4-Dimethoxy-2-pyridinemethanol

HRID 845537노트

반응식

HRID 845537 반응식
[OH-].[Na+].C([O:6][CH2:7][C:8]1[C:13]([O:14][CH3:15])=[C:12]([O:16][CH3:17])[CH:11]=[CH:10][N:9]=1)(=O)C>>[OH:6][CH2:7][C:8]1[C:13]([O:14][CH3:15])=[C:12]([O:16][CH3:17])[CH:11]=[CH:10][N:9]=1

참가 물질

3

반응물 2

HCID 14798Sodium HydroxideHCID 106085512-Acetoxymethyl-3,4-dimethoxypyridine

생성물 1

HCID 107258093,4-Dimethoxy-2-pyridinemethanol수율 96%

실험 절차

After adding 15 ml of 2N sodium hydroxide solution, 4.8 g of 2-acetoxymethyl-3,4-dimethoxypyridine are stirred vigorously at 80° C., whereupon a homogeneous solution forms from the initial two-phase mixture. After 2 hours, the solution is allowed to cool and is extracted five times with 30 ml of methylene chloride each time, the combined organic phases are washed twice with 5 ml of 0.3N sodium hydroxide solution each time, dried over potassium carbonate, filtered and concentrated and the distillation residue is stirred with petroleum ether. 3.6 g (96% of theory) of 2-hydroxymethyl-3,4-dimethoxy-pyridine are obtained as a colorless solid of m.p. 87°-89° C.

후처리

  1. temperatureto cool
  2. extractionis extracted five times with 30 ml of methylene chloride each time
  3. washthe combined organic phases are washed twice with 5 ml of 0.3N sodium hydroxide solution each time
  4. dry with materialdried over potassium carbonate
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3a9ea89d0a9c4fed80343e175ebbdb91
출처 데이터셋
uspto-grants-1988_07
특허 번호
US04758579

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