2,4-Dimethylpyridine → 2,4-Dimethylpyridine 1-oxide

HRID 77822

反応式

HRID 77822 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([CH3:7])=[CH:3][C:2]=1[CH3:8].ClC1C=C(C=CC=1)C(OO)=[O:14].S([O-])(O)=O.[Na+]>C(Cl)Cl>[CH3:8][C:2]1[CH:3]=[C:4]([CH3:7])[CH:5]=[CH:6][N+:1]=1[O-:14]

参加物

5

反応物 3

HCID 79362,4-DimethylpyridineHCID 70297m-Chloroperbenzoic acidHCID 23665763Sodium Bisulfite

生成物 1

HCID 707332,4-Dimethylpyridine 1-oxide収率 66.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2,4-lutidine (2.0 g, 18.7 mmol) in methylene chloride (100 mL) was added 3-chloroperoxybenzoic acid (5.07 g, 29.4 mmol), which was stirred for 20 minutes at room temperature. A small amount of saturated aqueous sodium hydrogen sulfite solution was added to the reaction solution, and the organic layer was separated after vigorous stirring. This organic layer was washed with 5 N aqueous sodium hydroxide solution (5.9 mL), and dried over anhydrous magnesium sulfate. The solvent was evaporated under a reduced pressure to obtain the title compound (1.54 g, 66.9%). The title compound was used in the following reaction without being purified.

後処理

  1. customthe organic layer was separated after vigorous stirring
  2. washThis organic layer was washed with 5 N aqueous sodium hydroxide solution (5.9 mL)
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under a reduced pressure

出典と根拠

ORDレコード
ord-89783daaca4d40328adeefc3033e8001
出典データセット
uspto-grants-2014_09
特許番号
US08841327B2

関連ノート

読み込み中…