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

HRID 265339노트

반응식

HRID 265339 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]>CO.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 887Methanol용매HCID 962Water용매

반응 조건

온도
20 °C

실험 절차

To a vigorously stirred solution, maintained under nitrogen, containing 277 mmol of 8-chloro-3,4-dihydro-2(1H)-naphthalenone in 350 ml of methanol and 170 ml of water are successively added 282 mmol of potassium cyanide and 290 mmol of ammonium chloride. After stirring for 48 hours at 20° C., the mixture is concentrated. The residue is taken up in ethyl acetate. This organic phase is washed with water and extracted with 1N hydrochloric acid. The acidic phases are basified with 35% sodium hydroxide and extracted with ethyl acetate. The expected product is obtained, in solid form, after drying and evaporating the organic phases.

후처리

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

출처 및 근거

ORD 기록
ord-c39b2ec7d2d5458e9de96f81a1c06a6f
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05648374

반응 노트

불러오는 중…