2-Phenylpyridine → 2-Phenylpyridine 1-Oxide

HRID 418051노트

반응식

HRID 418051 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 3024892-Phenylpyridine 1-Oxide수율 79.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-a44663e670ec4b0d82d1353224ea7e0e
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08093250B2

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