HRID69271

反应详情

EQUATION

反应方程式

HRID 69271 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

6-(6-Chloro-imidazo[1,2-b]pyridazin-3-ylmethyl)-7-fluoro-quinoline (Stage 173.1, 100 mg, 0.316 mmol), KF (92 mg, 1.581 mmol) and (S)-3-hydroxypyrrolidine (83 mg, 0.949 mmol) were suspended in NMP (1.5 mL). The RM was stirred at 170° C. for 1 h. The mixture was diluted with DCM/MeOH (95:5) and washed with water (2×). The aqueous phases were further extracted with DCM/MeOH (95:5) (2×). The combined organic layer was dried over Na2SO4, filtered and concentrated. The residue was crystallized in DCM to afford the title compound as a beige solid (tR 2.63 min (conditions 13), MH+=364).

WORKUP

后处理

  1. washwashed with water (2×)
  2. extractionThe aqueous phases were further extracted with DCM/MeOH (95:5) (2×)
  3. dry with materialThe combined organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was crystallized in DCM