Water → 1-Benzyl-3-methylpiperidin-4-ol

HRID 980873ノート

反応式

HRID 980873 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11](=[O:14])[CH:10]([CH3:15])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>CCOCC>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([OH:14])[CH:10]([CH3:15])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 962WaterHCID 5609651-Benzyl-3-methyl-4-piperidoneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 136114921-Benzyl-3-methylpiperidin-4-ol

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
25 °C

実験手順

Subsequently, 3.13 g of the 1-benzyl-3-methyl-4-piperidone obtained above was dissolved in 6 ml of ether. The solution was added dropwise to a suspension of 0.44 g of lithium aluminum hydride in 25 ml of ether over 5 minutes while maintaining the temperature at 24°-27° C. Then, the mixture was stirred at 25° C. for 10 minutes, and, 5 ml of water was added thereto under ice-cooling. The mixture was extracted with 30 ml of ether four times. The ether layer was washed with water, dried over anhydrous sodium sulfate and concentrated to obtain 3.17 g of an oily matter of 1-benzyl-4-hydroxy-3-methylpiperidine.

後処理

  1. temperaturewhile maintaining the temperature at 24°-27° C
  2. temperatureunder ice-cooling
  3. extractionThe mixture was extracted with 30 ml of ether four times
  4. washThe ether layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-d580ba0cf2e548029188e50f7859d8d9
出典データセット
uspto-grants-1987_01
特許番号
US04639522

反応ノート

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