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1-Benzyl-3-(3,4-dimethoxyphenyl)piperidin-3-ol → HCID 13066745、化合物

HRID 851131
ノート
印刷プレビュー

反応式

HRID 851131 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 130667441-Benzyl-3-(3,4-dimethoxyphenyl)piperidin-3-olHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 13066745HCID 13066745、化合物収率 74.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-880b19d1a9c043e9b3422722945db92d
出典データセット
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04382942

反応ノート

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