HRID69216

反应详情

EQUATION

反应方程式

HRID 69216 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(rac)-(6-Chloro-imidazo[1,2-b]pyridazin-3-yl)-(7-fluoro-quinolin-6-yl)-methanol (Stage 174.3, 329 g, 1.0 mmol) was dissolved in acetone (40 mL) and 2-iodoxybenzoic acid (45%, 1.245 g, 2.0 mmol) was added. The RM was heated to reflux for 3 h (suspension). The acetone was then removed under reduced pressure and the residue was taken up with water and 2 M NaOH. The beige suspension was filtered, washed with water and dried overnight under vacuum to afford the title compound as a beige powder (tR 4.31 min (conditions 3), MH+=327, 1H-NMR in DMSO-d6: 9.03 (d, 1H); 8.53 (d, 1H); 8.49-8.41 (m, 2H); 8.39 (s, 1H); 7.90 (d, 1H); 7.74 (d, 1H); 7.62 (dd, 1H)).

WORKUP

后处理

  1. temperatureThe RM was heated
  2. temperatureto reflux for 3 h (suspension)
  3. customThe acetone was then removed under reduced pressure
  4. filtrationThe beige suspension was filtered
  5. washwashed with water
  6. customdried overnight under vacuum