HRID1177407

反应详情

EQUATION

反应方程式

HRID 1177407 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A slurry of 2-(4-(1,3-dioxan-2-yl)-2-fluorophenyl)-5-chlorothiazolo[5,4-b]pyridine (5.00 g, 14.3 mmol) in 100 mL 1:1 THF/5N aq. HCl was heated in a sealed tube to 70° C. The thick orange mixture was cooled slightly and an additional 50 mL THF was added. The reaction mixture was sealed and heating continued. After 2 h, the reaction mixture was cooled and allowed to stir 3 days at ambient temperature. The reaction mixture was cooled and THF was removed in vacuo. The resulting yellow solid was collected by filtration through a frit, rinsing with water. The material was dried on the frit for several hours and dried in vacuo overnight to give 4-(5-chlorothiazolo[5,4-b]pyridine-2-yl)-3-fluorobenzaldehyde as a light yellow/orange solid. MS (ESI) m/z: calculated: 292.0: Observed: 292.9 (M++1).

WORKUP

后处理

  1. temperatureThe thick orange mixture was cooled slightly
  2. customThe reaction mixture was sealed
  3. temperatureheating
  4. temperaturethe reaction mixture was cooled
  5. temperatureThe reaction mixture was cooled
  6. customTHF was removed in vacuo
  7. filtrationThe resulting yellow solid was collected by filtration through a frit
  8. washrinsing with water
  9. customThe material was dried on the frit for several hours
  10. customdried in vacuo overnight