N-(3-Pyridylmethyl)Pyrrolidine → 3-(Pyrrolidin-1-ylmethyl)piperidine

HRID 1965943ノート

反応式

HRID 1965943 の反応式
[N:1]1([CH2:6][C:7]2[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1>C(O)(=O)C.O=[Pt]=O>[N:1]1([CH2:6][CH:7]2[CH2:12][CH2:11][CH2:10][NH:9][CH2:8]2)[CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

4

反応物 1

HCID 67786N-(3-Pyridylmethyl)Pyrrolidine

生成物 1

HCID 43418943-(Pyrrolidin-1-ylmethyl)piperidine

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 176Acetic Acid溶媒

実験手順

The educt 3-(1-pyrrolidinylmethyl)-pyridine (24.6 g) is taken up in 250 ml glacial acetic acid and hydrogenated with 2 g of PtO2 under 3 bar H2 at ambient temperature. The solution filtered off is evaporated down, combined with ice and made alkaline with solid KOH while cooling. After extracting three times with 250 ml of diethylether the crude product is dried with MgSO4. After the MgSO4 has been filtered off the solvent is eliminated and the amine is distilled in a water jet vacuum at a boiling point of 123° C.

後処理

  1. filtrationThe solution filtered off
  2. customis evaporated down
  3. temperaturewhile cooling
  4. extractionAfter extracting three times with 250 ml of diethylether the crude product
  5. dry with materialis dried with MgSO4
  6. filtrationAfter the MgSO4 has been filtered off the solvent
  7. distillationthe amine is distilled in a water jet vacuum at a boiling point of 123° C.

出典と根拠

ORDレコード
ord-a95b2330f7864603b6d06b26404b4ab6
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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