Potassium Cyanide → 2-Amino-2-cyano-5-methoxy-1,2,3,4-tetrahydronaphthalene

HRID 128713

반응식

HRID 128713 반응식
[C-:1]#[N:2].[K+].[Cl-].[NH4+:5].[CH3:6][O:7][C:8]1[CH:17]=[CH:16][CH:15]=[C:14]2[C:9]=1[CH2:10][CH2:11][C:12](=O)[CH2:13]2>C(O)C.O>[NH2:5][C:12]1([C:1]#[N:2])[CH2:11][CH2:10][C:9]2[C:14](=[CH:15][CH:16]=[CH:17][C:8]=2[O:7][CH3:6])[CH2:13]1

참가 물질

6

반응물 3

HCID 9032Potassium CyanideHCID 25517Ammonium ChlorideHCID 2591945-Methoxy-2-tetralone

생성물 1

HCID 99904312-Amino-2-cyano-5-methoxy-1,2,3,4-tetrahydronaphthalene

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

112 mmol of potassium cyanide and 116 mmol of ammonium chloride ate added successively to a solution, maintained under nitrogen and with stirring, containing 110 mmol of 5-methoxy-3,4-dihydronaphthalen-2(1H)-one in 90 ml of ethanol and 50 ml of water. The whole mixture is stirred for 20 hours at 20° C. and then concentrated under vacuum. The residue is taken up in 200 ml of ethyl acetate. This phase is then washed with water and extracted with 1N hydrochloric acid. The acid phase is basified with 35% sodium hydroxide solution and extracted with methyl acetate. The combined organic phases are dried and evaporated under vacuum and lead to the expected product in the solid form.

후처리

  1. temperaturemaintained under nitrogen
  2. stirringThe whole mixture is stirred for 20 hours at 20° C.
  3. concentrationconcentrated under vacuum
  4. washThis phase is then washed with water
  5. extractionextracted with 1N hydrochloric acid
  6. extractionextracted with methyl acetate
  7. customThe combined organic phases are dried
  8. customevaporated under vacuum and lead to the expected product in the solid form

출처 및 근거

ORD 기록
ord-ba8afc10f72a433885205de1993275b0
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05464859

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