Pyridine, 3-chloro-, 1-oxide → Pyridine, 3-methoxy-, 1-oxide

HRID 266912

반응식

HRID 266912 반응식
Cl[C:2]1[CH:3]=[N+:4]([O-:8])[CH:5]=[CH:6][CH:7]=1.[CH3:9][O-:10].[Na+]>CO>[CH3:9][O:10][C:2]1[CH:3]=[N+:4]([O-:8])[CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 123133Pyridine, 3-chloro-, 1-oxideHCID 10942334Sodium Methoxide

생성물 1

HCID 139850Pyridine, 3-methoxy-, 1-oxide수율 78%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 3-chloropyridine-N-oxide (5.3g, 40 mmol) and 25% NaOMe in MeOH (25 ml) was refluxed for 24 hours under an argon atmosphere. The solvent was removed under reduced pressure and the residue was treated with CH2Cl2 and water. The organic phase was separated and dried (Na2SO4) and the solvent removed to give a residue which was triturated with hexane to yield 4 g (78%) of product as a crystalline solid, m.p. 99°-101° C. The structural assignment is supported by the proton NMR spectrum.

후처리

  1. customThe solvent was removed under reduced pressure
  2. additionthe residue was treated with CH2Cl2 and water
  3. customThe organic phase was separated
  4. dry with materialdried (Na2SO4)
  5. customthe solvent removed
  6. customto give a residue which
  7. customwas triturated with hexane

출처 및 근거

ORD 기록
ord-1d234ef999c8460fb4c9a486bd20db82
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05652363

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