HRID69225

反应详情

EQUATION

反应方程式

HRID 69225 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-(5,7-difluoro-quinolin-6-yl)-methanone (Stage 182.3, 3.05 g, 8.41 mmol) was suspended in THF (65 mL) and the mixture was cooled down to 0° C. with an ice bath. Then the methylmagnesium bromide (1.4 M, 15.01 mL) was added slowly. The RM was stirred for 30 min and was then allowed to warm up to rt. After 2 h, it was quenched with a few mL of water. The solution was filtered. The solid residue was washed with water and the filtrate extracted with EtOAc twice. Then the organics were joined and washed with brine, dried over Na2SO4 and the solvent was removed. The crude was purified with DCM and MeOH by MPLC to give the title compound as a yellow solid (tR 0.9 min (conditions 2), MH+=361).

WORKUP

后处理

  1. temperatureto warm up to rt
  2. waitAfter 2 h
  3. customit was quenched with a few mL of water
  4. filtrationThe solution was filtered
  5. washThe solid residue was washed with water
  6. extractionthe filtrate extracted with EtOAc twice
  7. washwashed with brine
  8. dry with materialdried over Na2SO4
  9. customthe solvent was removed
  10. customThe crude was purified with DCM and MeOH by MPLC