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Water → 4-(Diethylamino)-2-(naphthalen-1-yl)butanenitrile

HRID 620184
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HRID 620184 반응식
[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.Cl[CH2:17][CH2:18][N:19]([CH2:22][CH3:23])[CH2:20][CH3:21].O>C1C=CC=CC=1>[CH2:18]([N:19]([CH2:22][CH2:23][CH:13]([C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=1)[C:14]#[N:15])[CH2:20][CH3:21])[CH3:17]
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참가 물질

6

반응물 4

HCID 962WaterHCID 85961-NaphthaleneacetonitrileHCID 13364Diethylaminoethyl chlorideHCID 24533Sodium amide

생성물 1

HCID 173954-(Diethylamino)-2-(naphthalen-1-yl)butanenitrile

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

7 g of sodium amide are added in small quantities to 27.11 g of 1-naphthylacetonitrile in 210 ml of anhydrous benzene. The mixture is heated for 2 hours to reflux and 22 g of 2-chlorodiethylaminoethane are added, the heating being continued to reflux for another two and a half hours. Then, the mixture is cooled and 200 ml of water are added. After decanting, the organic phase is extracted by HCl at 10%. The aqueous phase is washed in ether, neutralized with NaOH at 10%, then extracted with ether. After evaporation of the solvents, a red oil is obtained, which is distilled in vacuo.

후처리

  1. temperatureThe mixture is heated for 2 hours
  2. temperatureto reflux
  3. temperatureto reflux for another two and a half hours
  4. temperatureThen, the mixture is cooled
  5. customAfter decanting
  6. extractionthe organic phase is extracted by HCl at 10%
  7. washThe aqueous phase is washed in ether
  8. extractionextracted with ether
  9. customAfter evaporation of the solvents
  10. customa red oil is obtained
  11. distillationwhich is distilled in vacuo

출처 및 근거

ORD 기록
ord-4f69d616f8da4d33875e10cd41f600d6
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04820717

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