Water → HCID 18691144、化合物

HRID 376318

反応式

HRID 376318 の反応式
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][N:3]=1.[CH3:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[C:19](=O)[CH2:20]Br.C(=O)(O)[O-].[Na+].O>C(O)C>[CH3:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[C:19]1[N:1]=[C:2]2[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[CH:5]=[CH:4][N:3]2[CH:20]=1

参加物

6

反応物 4

HCID 962WaterHCID 737421-IsoquinolinamineHCID 516892Sodium BicarbonateHCID 124306762-Bromo-2'-methylacetophenone

生成物 1

HCID 18691144HCID 18691144、化合物収率 81.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 3.0 g of 1-aminoisoquinoline, 6.7 g of 2'-methyl-2-bromoacetophenone and 17.5 g of sodium bicarbonate in 50 ml of ethanol was refluxed for 2 hours. After being cooled, the reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with water and saturated saline, and dried over anhydrous magnesium sulfate. The drying agent was removed by filtration, and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel and recrystallized from dichloromethane/petroleum ether to give 4.4 g of the title compound as pale brown prisms.

後処理

  1. temperaturewas refluxed for 2 hours
  2. temperatureAfter being cooled
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water and saturated saline
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe drying agent was removed by filtration
  7. customthe solvent was removed under reduced pressure
  8. customThe residue was purified by column chromatography on silica gel
  9. customrecrystallized from dichloromethane/petroleum ether

出典と根拠

ORDレコード
ord-3964bf73098b47a1a5f31d79cdefaabc
出典データセット
uspto-grants-2000_02
特許番号
US06020342

関連ノート

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