1-Methyl-4-(nitromethyl)piperidin-4-ol → 4-(Aminomethyl)-1-methylpiperidin-4-ol

HRID 1469330

反応式

HRID 1469330 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][C:5]([CH2:9][N+:10]([O-])=O)([OH:8])[CH2:4][CH2:3]1>C(O)C.[OH-].[Pd+2].[OH-]>[NH2:10][CH2:9][C:5]1([OH:8])[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1

参加物

4

反応物 1

HCID 2733771-Methyl-4-(nitromethyl)piperidin-4-ol

生成物 1

HCID 64842624-(Aminomethyl)-1-methylpiperidin-4-ol収率 106.3%

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 702Ethanol溶媒

実験手順

Palladium hydroxide (2.3 g of 20% on carbon) was added to a solution of 1-methyl-4-nitromethylpiperidin-4-ol (11.57 g) in ethanol (120 mL). The mixture was placed under hydrogen pressure (50 psi, 3.4×105 Pa) on a Parr apparatus for 55 hours. The reaction mixture was filtered through a layer of CELITE filter aid and the filter cake was rinsed with methanol (100 mL). The filtrate was concentrated under reduced pressure to provide 10.18 g of 4-aminomethyl-1-methylpiperidin-4-ol as a thick oil.

後処理

  1. customfor 55 hours
  2. filtrationThe reaction mixture was filtered through a layer of CELITE
  3. filtrationfilter aid
  4. washthe filter cake was rinsed with methanol (100 mL)
  5. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-1732c157d53842e9b4f3613995a655d2
出典データセット
uspto-grants-2015_04
特許番号
US09006264B2

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