2-Chloro-5-nitropyrimidine → 2-Methoxy-5-nitropyrimidine

HRID 450179

반응식

HRID 450179 반응식
[CH3:1][O-:2].[Na+].Cl[C:5]1[N:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][N:6]=1>CO>[CH3:1][O:2][C:5]1[N:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][N:6]=1

참가 물질

4

반응물 2

HCID 825442-Chloro-5-nitropyrimidineHCID 10942334Sodium Methoxide

생성물 1

HCID 3529002-Methoxy-5-nitropyrimidine수율 134.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of sodium methoxide (0.090 g of sodium) in MeOH (12 mL) was added 0.486 g (3.03 mmol) of 2-chloro-5-nitropyrimidine, and the mixture was heated under reflux for 1 hr. After cooling, the mixture was concentrated in vacuo, extracted with EtOAc, and washed with water. The aqueous layer was extracted with CHCl3 and the combined organic layers were dried (Na2SO4), and concentrated, to give 0.347 g (75% yield) of 2-methoxy-5-nitropyrimidine as a yellow powder: 1H NMR (CDCl3) δ9.31 (s, 2H), 4.17 (s, 3H); LCMS (APCI+) m/z: 156 (MH+, 100%).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1 hr
  3. temperatureAfter cooling
  4. concentrationthe mixture was concentrated in vacuo
  5. extractionextracted with EtOAc
  6. washwashed with water
  7. extractionThe aqueous layer was extracted with CHCl3
  8. dry with materialthe combined organic layers were dried (Na2SO4)
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-160f4f9dca0f416a938b965dced57a0a
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486939B2

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