Ammonia → 1-Isoquinolinamine, 7-methoxy-

HRID 1008548

반응식

HRID 1008548 반응식
[NH3:1].Cl[C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([O:13][CH3:14])[CH:11]=2)[CH:6]=[CH:5][N:4]=1>C(O)C>[CH3:14][O:13][C:10]1[CH:11]=[C:12]2[C:7]([CH:6]=[CH:5][N:4]=[C:3]2[NH2:1])=[CH:8][CH:9]=1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 222501811-Chloro-7-methoxyisoquinoline

생성물 1

HCID 226656441-Isoquinolinamine, 7-methoxy-

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
170 °C

실험 절차

Liquid ammonia (220 mL) was added to a solution of 32.8 g of 1-chloro-7-methoxy-isoquinoline in 420 mL of ethanol in a steel vessel Nitrogen was pressed upon until an initial pressure of 20 atm. was obtained. This reaction mixture was heated for 2 days at 170° C. The solvent was removed in vacuo and the residue dissolved in water. The pH value was adjusted to pH 10 by adding aqueous sodium carbonate solution, followed by extraction with ethyl acetate. The organic extract was washed with brine and dried (Na2SO4). Evaporation of the solvent in vacuo gave pure 7-methoxy-isoquinoline-1-ylamine as a white solid. Yield 24.0 g (81%); m.p. 128-130° C.

후처리

  1. customwas obtained
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue dissolved in water
  4. additionby adding aqueous sodium carbonate solution
  5. extractionfollowed by extraction with ethyl acetate
  6. extractionThe organic extract
  7. washwas washed with brine
  8. dry with materialdried (Na2SO4)
  9. customEvaporation of the solvent in vacuo

출처 및 근거

ORD 기록
ord-b729ed7552204b54a3939278f18e02bc
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06797710B2

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