HRID1778148

反应详情

EQUATION

反应方程式

HRID 1778148 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To a solution of methyl 6-amino-5-({3-[(3-methyl-2-furoyl)amino]phenyl}ethynyl)nicotinate, (1.82 g, 4.85 mmol, 1 eq) in MeOH—H2O (100 mL, 3:1) at RT was added potassium hydroxide (2.72 g, 10 eq) with stirring. The mixture was heated at 65° C. for 2 hours and a brown solution was observed at this time. The reaction mixture was concentrated to remove most of the methanol. The resulting solution was cooled to 0° C. and concentrated HCl was added until the pH was around 3 at which time a white precipitates formed. The solid which had formed was collected by filtration, rinsed with water, and dried to give the title compound as a white solid (1.75 g).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. customto remove most of the methanol
  3. temperatureThe resulting solution was cooled to 0° C.
  4. additionconcentrated HCl was added until the pH was around 3 at which time
  5. customa white precipitates
  6. customformed
  7. customThe solid which had formed
  8. filtrationwas collected by filtration
  9. washrinsed with water
  10. customdried