2-Phenylpyridine → 2-Phenylpyridine 1-Oxide

HRID 418051

反応式

HRID 418051 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[C:12]1([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C([O-])(O)=O.[Na+]>C(Cl)Cl>[C:12]1([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][N+:19]=2[O-:9])[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

参加物

5

反応物 3

HCID 138872-PhenylpyridineHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium Bicarbonate

生成物 1

HCID 3024892-Phenylpyridine 1-Oxide収率 79.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3-chloroperbenzoic acid (19 g) was added portionwise to an ice-cold solution of 2-phenylpyridine (10 g) in DCM (30 ml). The mixture was allowed to warm to RT and was stirred at RT for 4 h. 100 ml of a NaHCO3 solution were added to the reaction mixture and the phases were separated. The aq. phase was further extracted with DCM and the combined org. phases were washed with an aq. NaHSO3 (40%) solution and evaporated off. Recrystallisation (EA) afforded 8.77 g of the desired compound.

後処理

  1. customthe phases were separated
  2. extractionThe aq. phase was further extracted with DCM
  3. washphases were washed with an aq. NaHSO3 (40%) solution
  4. customevaporated off
  5. customRecrystallisation (EA)

出典と根拠

ORDレコード
ord-a44663e670ec4b0d82d1353224ea7e0e
出典データセット
uspto-grants-2012_01
特許番号
US08093250B2

関連ノート

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