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

HRID 266912

反応式

HRID 266912 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 139850Pyridine, 3-methoxy-, 1-oxide収率 78%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1d234ef999c8460fb4c9a486bd20db82
出典データセット
uspto-grants-1997_07
特許番号
US05652363

関連ノート

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