HCID 12926609、化合物 → SR 57227A
反応式
C([NH:4][CH:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([Cl:17])[N:12]=2)[CH2:7][CH2:6]1)(=O)C>Cl>[NH2:4][CH:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([Cl:17])[N:12]=2)[CH2:7][CH2:6]1参加物
3
実験手順
A solution of 0.482 mole of 4-acetamido-1-(6-chloro-2-pyridyl)piperidine in 610 ml of 6 N hydrochloric acid is heated at reflux for 8 hours, then the reaction mixture is cooled and concentrated under reduced pressure. The residue is treated with 4 N sodium hydroxide up to a clearly basic pH and the oil which separates is extracted with diethyl ether. The organic phase is washed with water, dried over anhydrous sodium sulfate and evaporated to dryness. The oily residue is crystallised by diisopropylic ether. 4-amino-1-(6-chloro-2-pyridyl)piperidine is thus obtained; m.p. 36° to 38° C.
後処理
- temperatureat reflux for 8 hours
- temperaturethe reaction mixture is cooled
- concentrationconcentrated under reduced pressure
- additionThe residue is treated with 4 N sodium hydroxide up to a clearly basic pH
- extractionthe oil which separates is extracted with diethyl ether
- washThe organic phase is washed with water
- dry with materialdried over anhydrous sodium sulfate
- customevaporated to dryness
- customThe oily residue is crystallised by diisopropylic ether
出典と根拠
- ORDレコード
- ord-c6372d8c214444b3acdbfac197ae593c
- 出典データセット
- uspto-grants-1983_10
- 特許番号
- US04409228
反応ノート
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