Ammonia → 1-Isoquinolinamine, 7-methoxy-

HRID 636967ノート

反応式

HRID 636967 の反応式
[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

参加物

4

反応物 2

HCID 222AmmoniaHCID 222501811-Chloro-7-methoxyisoquinoline

生成物 1

HCID 226656441-Isoquinolinamine, 7-methoxy-

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
170 °C

実験手順

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-isoquinolin-1-ylamine as a white solid. Yield 24.0 g (81%); m.p. 128-130° C.

後処理

  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

出典と根拠

ORDレコード
ord-2c4a83e88f0947c2bc65322095e8f7d4
出典データセット
uspto-grants-2001_02
特許番号
US06194409B1

反応ノート

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