HRID1942098

反应详情

EQUATION

反应方程式

HRID 1942098 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

6-chloro-3-((4,6-difluoro-1-methyl-1H-indazol-5-yl)methyl)imidazo[1,2-b]pyridazine (Intermediate T, 40.0 mg, 0.12 mmol), KF (34.8 mg, 0.6 mmol) and 1-acetylpiperazine (46.1 mg, 0.36 mmol) were suspended in NMP (0.3 mL). The RM was stirred at 180° C. for 3 h. The mixture was diluted with EtOAc and washed with NaHCO3 10% (2×) and water (4×). The combined organic layers were dried over Na2SO4, filtered and concentrated. The residue was purified by flash chromatography and afforded the title compound as a light brown foam (tR 3.72 min (conditions 5), MH+=426.3, 1H-NMR in DMSO-d6: 8.16 (s, 1H); 7.80 (d, 1H); 7.46 (d, 1H); 7.27 (s, 1H); 7.10 (d, 1H); 4.27 (s, 2H); 3.98 (s, 3H); 3.50 (s, 6H); 3.44 (m, 2H); 2.03 (s, 3H)).

WORKUP

后处理

  1. washwashed with NaHCO3 10% (2×) and water (4×)
  2. dry with materialThe combined organic layers were dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by flash chromatography