N,N-dimethyl-2-[methyl-(2-pyridine-4-yl-ethyl)-amino]-acetamide → N,N-dimethyl-2-[methyl-(2-piperidin-4-yl-ethyl)-amino]-acetamide

HRID 1965945ノート

反応式

HRID 1965945 の反応式
[CH3:1][N:2]([CH3:16])[C:3](=[O:15])[CH2:4][N:5]([CH3:14])[CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=1>C(O)(=O)C.CCOCC.O=[Pt]=O>[CH3:16][N:2]([CH3:1])[C:3](=[O:15])[CH2:4][N:5]([CH3:14])[CH2:6][CH2:7][CH:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1

参加物

5

反応物 1

HCID 21081298N,N-dimethyl-2-[methyl-(2-pyridine-4-yl-ethyl)-amino]-acetamide

生成物 1

HCID 21081297N,N-dimethyl-2-[methyl-(2-piperidin-4-yl-ethyl)-amino]-acetamide

試薬・触媒・溶媒 3

HCID 345198Adams' catalyst触媒HCID 176Acetic Acid溶媒HCID 3283Diethyl Ether溶媒

実験手順

Of the crude N,N-dimethyl-2-[methyl-(2-pyridine-4-yl-ethyl)-amino]-acetamide, 44 g are dissolved in 500 ml of glacial acetic acid and hydrogenated with 4 g of PtO2 at ambient temperature under 3 bar H2. After the catalyst has been removed by suction filtering the filtrate is evaporated down. The residue is made alkaline with 50% potassium hydroxide solution while cooling with ice and the product obtained is taken up in ether. The ether solution is dried over sodium sulphate, filtered and the solution is evaporated down. The product is left as a yellow oil. Yield: 42 g

後処理

  1. customAfter the catalyst has been removed by suction
  2. filtrationfiltering the filtrate
  3. customis evaporated down
  4. temperaturewhile cooling with ice
  5. customthe product obtained
  6. dry with materialThe ether solution is dried over sodium sulphate
  7. filtrationfiltered
  8. customthe solution is evaporated down
  9. waitThe product is left as a yellow oil

出典と根拠

ORDレコード
ord-05c0a3db95d94e0f9fae11e3e39eced8
出典データセット
uspto-grants-2013_04
特許番号
US08420630B2

反応ノート

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