Potassium Cyanide → 2-Amino-2-cyano-8-chloro-1,2,3,4-tetrahydronaphthalene

HRID 265338

반응식

HRID 265338 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[CH2:10][C:9](=O)[CH2:8][CH2:7]2.[C-:13]#[N:14].[K+].[Cl-].[NH4+:17]>C(O)C.O>[NH2:17][C:9]1([C:13]#[N:14])[CH2:8][CH2:7][C:6]2[C:11](=[C:2]([Cl:1])[CH:3]=[CH:4][CH:5]=2)[CH2:10]1

참가 물질

6

반응물 3

HCID 9032Potassium CyanideHCID 25517Ammonium ChlorideHCID 46232698-Chloro-1,2,3,4-tetrahydronaphthalen-2-one

생성물 1

HCID 118203212-Amino-2-cyano-8-chloro-1,2,3,4-tetrahydronaphthalene

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
20 °C

실험 절차

To a vigorously stirred solution, maintained under nitrogen, containing 43 mmol of 8-chloro-3,4-dihydro-2(1H)-naphthalenone in 60 ml of ethanol and 30 ml of water are successively added 44 mmol of potassium cyanide and 44 mmol of ammonium chloride. After stirring for 20 hours at 20° C., the mixture is concentrated under vacuum and the residue is taken up in 80 ml of ethyl acetate. This organic phase is washed with water and is then extracted with 1N hydrochloric acid. The aqueous phase is basified with 35% sodium hydroxide and extracted with ethyl acetate. The expected product is obtained after drying and evaporation of the organic phase as a solid.

후처리

  1. temperatureTo a vigorously stirred solution, maintained under nitrogen
  2. concentrationthe mixture is concentrated under vacuum
  3. washThis organic phase is washed with water
  4. extractionis then extracted with 1N hydrochloric acid
  5. extractionextracted with ethyl acetate

출처 및 근거

ORD 기록
ord-9de5389e5f984306a0a0ef9a71726e91
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05648374

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