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1-Naphthaleneacetonitrile → 2-(Naphthalen-1-yl)-4-(piperidin-1-yl)butanenitrile

HRID 620186
ノート
印刷プレビュー

反応式

HRID 620186 の反応式
[NH2-].[Na+].[C:3]1([CH2:13][C:14]#[N:15])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=1.[N:16]1([CH2:22][CH2:23]Cl)[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1>CCOCC.O>[C:3]1([CH:13]([CH2:23][CH2:22][N:16]2[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)[C:14]#[N:15])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 85961-NaphthaleneacetonitrileHCID 24533Sodium amideHCID 748271-(2-Chloroethyl)piperidine

生成物 1

HCID 141712-(Naphthalen-1-yl)-4-(piperidin-1-yl)butanenitrile

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

8.2 g of sodium amide are added in small quantities on a solution of 33.4 g of 1-naphthyl acetonitrile in 450 ml of anhydrous ether. The mixture is heated for 2 hours to reflux, then 29.5 g of 2-piperidino-1-chloroethane are added, a heating to reflux is repeated for 5 hours. The mixture is then cooled, poured in water, and the organic phase is extracted 3 times with 600 ml of hydrochloric acid at 10%. The aqueous phase is washed with ether and neutralized with soda at 30%. The decanting oil is extracted, washed with sodium chloride-saturated water and dried over magnesium sulphate. After evaporation of the solvent, the resulting oil is distilled under reduced pressure (vane pump).

後処理

  1. temperatureThe mixture is heated for 2 hours
  2. temperatureto reflux
  3. temperaturea heating to reflux
  4. temperatureThe mixture is then cooled
  5. extractionthe organic phase is extracted 3 times with 600 ml of hydrochloric acid at 10%
  6. washThe aqueous phase is washed with ether and neutralized with soda at 30%
  7. extractionThe decanting oil is extracted
  8. washwashed with sodium chloride-saturated water
  9. dry with materialdried over magnesium sulphate
  10. customAfter evaporation of the solvent
  11. distillationthe resulting oil is distilled under reduced pressure (vane pump)

出典と根拠

ORDレコード
ord-362806f4ff914b018c2cef575c633584
出典データセット
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04820717

反応ノート

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