HRID1942075

反应详情

EQUATION

反应方程式

HRID 1942075 的结构方程式

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

(rac)-6-[1-(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-ethyl]-5,7-difluoro-quinoline (Intermediate C, 55 mg, 0.160 mmol), KF (46.3 mg, 0.798 mmol), 3-methylpiperazine (54.6 mg, 0.479 mmol) were suspended in NMP (532 μL). The RM was stirred at 180° C. for 16 h. The mixture was purified by preparative UPLC with acetonitrile and water (+0.1% TFA) The fractions were collected and acetonitrile was removed. It was taken up with EtOAc/MeOH (9/1) and washed with 5% Na2CO3 solution and brine. The organic layer was dried over sodium sulfate and the solvent was removed. A brown solid was obtained (tR 0.9 min (conditions 4), MH+=423)

WORKUP

后处理

  1. customThe mixture was purified by preparative UPLC with acetonitrile and water (+0.1% TFA) The fractions
  2. customwere collected
  3. customacetonitrile was removed
  4. washwashed with 5% Na2CO3 solution and brine
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. customthe solvent was removed
  7. customA brown solid was obtained (tR 0.9 min (conditions 4), MH+=423)