Hydrogen Bromide → HCID 136055524、化合物

HRID 2101044

反応式

HRID 2101044 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[C:18]2[C:13](=[CH:14][C:15]([O:19]C)=[CH:16][CH:17]=2)[CH:12]=[C:11]([NH:21][C:22]2[CH:26]=[C:25]([CH3:27])[NH:24][N:23]=2)[N:10]=1.Br>C(O)(=O)C>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[C:18]2[C:13](=[CH:14][C:15]([OH:19])=[CH:16][CH:17]=2)[CH:12]=[C:11]([NH:21][C:22]2[CH:26]=[C:25]([CH3:27])[NH:24][N:23]=2)[N:10]=1

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 23633788[1-(2,4-difluoro-phenyl)-6-methoxy-isoquinolin-3-yl]-(5-methyl-1H-pyrazol-3-yl)-amine

生成物 1

HCID 136055524HCID 136055524、化合物収率 8.7%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
180 °C

実験手順

To a solution of [1-(2,4-difluoro-phenyl)-6-methoxy-isoquinolin-3-yl]-(5-methyl-1H-pyrazol-3-yl)-amine (11.0 g) in 10 mL acetic acid was added hydrobromic acid (1 mL, 40%). The mixture was heated at 180° C. for 30 min under microwave irradiation. After cooling, most of the solvent was removed under reduced pressure, the residue was dissolved in 100 mL of ethyl acetate and washed with saturated sodium bicarbonate. The organic phase was dried with anhydrous sodium sulfate and concentrated to give an oil (0.92 g), which was used for the next reaction without further purification. (LC-MS m/e 353 MH+).

後処理

  1. temperatureAfter cooling, most of the solvent
  2. customwas removed under reduced pressure
  3. dissolutionthe residue was dissolved in 100 mL of ethyl acetate
  4. washwashed with saturated sodium bicarbonate
  5. dry with materialThe organic phase was dried with anhydrous sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-651daadcade84d478828c1227c5f054e
出典データセット
uspto-grants-2009_08
特許番号
US07572809B2

関連ノート

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