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alpha-(3,4-Dimethoxy-5-nitrophenyl)-2-pyridinemethanol → 3,4-Dimethoxy-5-nitrophenyl 2-pyridyl ketone

HRID 274500
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HRID 274500 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:14]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][N:17]=2)[OH:15])[CH:6]=[C:7]([N+:11]([O-:13])=[O:12])[C:8]=1[O:9][CH3:10]>CC(C)=O.[O-2].[O-2].[Mn+4]>[N:17]1[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=1[C:14]([C:5]1[CH:6]=[C:7]([N+:11]([O-:13])=[O:12])[C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=1)=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 21459111alpha-(3,4-Dimethoxy-5-nitrophenyl)-2-pyridinemethanol

생성물 1

HCID 179777233,4-Dimethoxy-5-nitrophenyl 2-pyridyl ketone

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 180Acetone용매

실험 절차

7 g of manganese dioxide and added portionwise to 4.0 g of α-(3,4-dimethoxy-5-nitrophenyl)-2-pyridine-methanol dissolved in 100 ml of acetone while constantly heating under reflux over a period of 2.5 hours. Thereupon, the mixture is heated under reflux for an additional 2 hours. The manganese salts are subsequently filtered and the residue obtained after evaporation is recrystallized from ether/hexane. There is obtained 3,4-dimethoxy-5-nitrophenyl 2-pyridyl ketone of m.p. 113°.

후처리

  1. temperaturewhile constantly heating
  2. temperatureunder reflux over a period of 2.5 hours
  3. temperatureThereupon, the mixture is heated
  4. temperatureunder reflux for an additional 2 hours
  5. filtrationThe manganese salts are subsequently filtered
  6. customthe residue obtained
  7. customafter evaporation
  8. customis recrystallized from ether/hexane

출처 및 근거

ORD 기록
ord-793faa31426341a1adbfcfbdeb12836b
출처 데이터셋
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05389653

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