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1-Benzyl-3-(3,4-dimethoxyphenyl)piperidin-3-ol → HCID 13066745, 화합물

HRID 851131
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HRID 851131 반응식
C([N:8]1[CH2:13][CH2:12][CH2:11][C:10]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[C:17]([O:23][CH3:24])[CH:16]=2)([OH:14])[CH2:9]1)C1C=CC=CC=1.[H][H]>C(O)C>[CH3:24][O:23][C:17]1[CH:16]=[C:15]([C:10]2([OH:14])[CH2:11][CH2:12][CH2:13][NH:8][CH2:9]2)[CH:20]=[CH:19][C:18]=1[O:21][CH3:22]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 130667441-Benzyl-3-(3,4-dimethoxyphenyl)piperidin-3-olHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 13066745HCID 13066745, 화합물수율 74.6%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
100 °C

실험 절차

A mixture of 5 g of 10% palladized carbon and a solution of 9.8 g of N-benzyl-3-(3,4-dimethoxyphenyl)-3-hydroxy-piperidine [described in French patent No. 2,310,761] in 100 ml of ethanol was placed in an autoclave and hydrogen was introduced to obtain a pressure of 50 kg/cm2. The autoclave was sealed and was heated at 100° C. and the hydrogen pressure stabilized at 65 kg/cm2. The mixture was stirred at 100° C. for 32 hours and was then cooled and filtered. The filtrate was evaporated to dryness under reduced pressure and the residue was chromatographed over silica gel. Elution with a 75-20-5 chloroform-methanol-triethylamine mixture yielded 5.3 g of 3-(3,4-dimethoxyphenyl)-3-hydroxy-piperidine.

후처리

  1. additionA mixture of 5 g of 10%
  2. additionwas introduced
  3. customto obtain a pressure of 50 kg/cm2
  4. customThe autoclave was sealed
  5. temperaturewas then cooled
  6. filtrationfiltered
  7. customThe filtrate was evaporated to dryness under reduced pressure
  8. customthe residue was chromatographed over silica gel
  9. washElution with a 75-20-5 chloroform-methanol-triethylamine mixture

출처 및 근거

ORD 기록
ord-880b19d1a9c043e9b3422722945db92d
출처 데이터셋
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04382942

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