Hydrogen Bromide → HCID 136055524, 화합물

HRID 2101044

반응식

HRID 2101044 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 136055524HCID 136055524, 화합물수율 8.7%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
180 °C

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-651daadcade84d478828c1227c5f054e
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07572809B2

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