HRID1367281

反应详情

EQUATION

反应方程式

HRID 1367281 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1H-Pyrrolo[2,3-b]pyridine (1, 0.455 g, 3.85 mmol) and 6-chloro-2-methoxypyridine-3-carbaldehyde (26, 0.661 g, 3.85 mmol) was added methanol (10 mL) followed by potassium hydroxide (0.310 g, 5.52 mmol). The reaction was allowed to stir at room temperature overnight. The reaction was extracted with diethyl ether/ethyl acetate and water. The organic layer was separated, dried over anhydrous magnesium sulfate, filtered and volatiles were removed by rotary evaporation to provide a solid that was treated with dichloromethane and stored in a freezer overnight. The white solid was collected by vacuum filtration and dried in vacuo to give 613 mg of compound 27 (2.12 mmol, 55%). MS(ESI) [M+H+]+=290.1.

WORKUP

后处理

  1. extractionThe reaction was extracted with diethyl ether/ethyl acetate and water
  2. customThe organic layer was separated
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customvolatiles were removed by rotary evaporation
  6. customto provide a solid
  7. waitstored in a freezer overnight
  8. filtrationThe white solid was collected by vacuum filtration
  9. customdried in vacuo