Hydrochloric Acid → (1-Benzyl-4-piperidyl)methanamine

HRID 54556

反応式

HRID 54556 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([C:14](=O)[NH2:15])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl>O1CCCC1>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][NH2:15])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 7831561-Benzylpiperidine-4-carboxamide

生成物 1

HCID 1514444(1-Benzyl-4-piperidyl)methanamine収率 59.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 1-benzyl-4-carbamoylpiperidine (2.5 g) in tetrahydrofuran (10 ml) was added dropwise to 1N solution of diborane-tetrahydrofuran complex in tetrahydrofuran (34.3 ml) at 0° C. and then the mixture was refluxed for 3 hours. After cooling to room temperature, 6N hydrochloric acid (10 ml) was added thereto. The mixture was stirred overnight and concentrated in vacuo. The residue was dissolved in ethyl acetate and made basic with 5N sodium hydroxide. The separated organic layer was washed with water and brine and dried over magnesium sulfate, and evaporated in vacuo to give (1-benzylpiperidin-4-yl)methylamine (1.4 g) as an oil.

後処理

  1. temperaturethe mixture was refluxed for 3 hours
  2. concentrationconcentrated in vacuo
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washThe separated organic layer was washed with water and brine
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-018b6baf30414d4e9bc50e685a97c250
出典データセット
uspto-grants-1997_04
特許番号
US05622976

関連ノート

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