HRID872846

反应详情

EQUATION

反应方程式

HRID 872846 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a flask containing a mixture of ethyl imidazo[1,2-a]pyridine-2-carboxylate (1 g, 5.26 mmol), THF (5 ml) and water (5 ml), lithium hydroxide (0.378 g, 15.77 mmol) was added and stirred overnight at RT. The pH of the reaction mixture was adjusted to 2 with 2 M HCl and THF was evaporated. The remaining water phase was extracted with ethyl acetate and the combined ethyl acetate phases were dried. The product had precipitated into the water phase. Water was evaporated, and the remaining solid recrystallized from methanol. The product was used as a salt in the next step. 1H-NMR (400 MHz; DMSO-d6): δ 7.23-7.26 (m, 1H), 7.63-7.70 (m, 1H), 7.76 (dd, 1H), 8.72 (s, 1H), 8.73-8.77 (m, 1H).

WORKUP

后处理

  1. additionInto a flask containing
  2. additionwas added
  3. customwas evaporated
  4. extractionThe remaining water phase was extracted with ethyl acetate
  5. dry with materialthe combined ethyl acetate phases were dried
  6. customThe product had precipitated into the water phase
  7. customWater was evaporated
  8. customthe remaining solid recrystallized from methanol