Water → 2-Methoxy-4-methyl-5-nitropyridine

HRID 53528

반응식

HRID 53528 반응식
[CH3:1][O-:2].[Na+].Cl[C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([N+:12]([O-:14])=[O:13])=[CH:7][N:6]=1.O>CO>[CH3:1][O:2][C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([N+:12]([O-:14])=[O:13])=[CH:7][N:6]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 3453642-Chloro-4-methyl-5-nitropyridineHCID 10942334Sodium Methoxide

생성물 1

HCID 2431692-Methoxy-4-methyl-5-nitropyridine수율 55.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium methoxide (26.1 g) was added to a solution of 2-chloro-4-methyl-5-nitropyridine (19.0 g) in methanol (100 ml) and the resulting mixture was refluxed for 12 hours. Upon cooling, the mixture was poured over water (1 L), and the product was extracted with ethyl acetate and washed with water. The organic phase was dried (anhydrous magnesium sulfate) and concentrated, and the residue dissolved in hot ether and filtered. Crystallization from ether provided 10.2 g of the title compound, suitable for use in the next reaction.

후처리

  1. temperaturethe resulting mixture was refluxed for 12 hours
  2. temperatureUpon cooling
  3. extractionthe product was extracted with ethyl acetate
  4. washwashed with water
  5. dry with materialThe organic phase was dried (anhydrous magnesium sulfate)
  6. concentrationconcentrated
  7. dissolutionthe residue dissolved in hot ether
  8. filtrationfiltered
  9. customCrystallization from ether

출처 및 근거

ORD 기록
ord-3d639581d26c44ddb7f10dbba34ccf92
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05620974

연결된 노트

불러오는 중…