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2-(2,4-dimethoxyphenyl)pyridine → HCID 135433735, 화합물

HRID 322944
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HRID 322944 반응식
C[O:2][C:3]1[CH:8]=[C:7]([O:9]C)[CH:6]=[CH:5][C:4]=1[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=1>Cl.N1C=CC=CC=1.ClCCl>[OH:2][C:3]1[CH:8]=[C:7]([OH:9])[CH:6]=[CH:5][C:4]=1[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=1
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참가 물질

4

반응물 1

HCID 108463432-(2,4-dimethoxyphenyl)pyridine

생성물 1

HCID 135433735HCID 135433735, 화합물수율 65.7%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 10176127Pyridinium chloride용매

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온도
160 °C

실험 절차

A mixture of 2-(2,4-dimethoxyphenyl)pyridine (14 g) in pyridine hydrochloride (121 g) is heated to 160° C. and the resulting melt is heated at 160° C. for 7 hours. The mixture is then cooled, diluted with dichloromethane, washed with hydrochloric acid (2 M) and water, dried and evaporated. The residual oil is subjected to flash chromatography on silica gel, eluting with a mixture of pentane and ethyl acetate (1:1 v/v), to give 2-(2,4-dihydroxyphenyl)pyridine (8.0 g) in the form of a solid, m.p. 170-172° C. [NMR(CDCl3):- 6.3(1H,s),6.4(1H,d),7.3(1H,m), 7.8(1H,d),7.9(1H,t),8.0(1H,d),8.5(1H,d).

후처리

  1. temperaturethe resulting melt is heated at 160° C. for 7 hours
  2. temperatureThe mixture is then cooled
  3. washwashed with hydrochloric acid (2 M) and water
  4. customdried
  5. customevaporated
  6. washeluting with a mixture of pentane and ethyl acetate (1:1 v/v)

출처 및 근거

ORD 기록
ord-a34cfc667f27469988281fcb680c67ad
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06211234B1

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