HRID868999

反应详情

EQUATION

反应方程式

HRID 868999 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of methyl 3-methylimidazo[2,1-f][1,6]naphthyridine-2-carboxylate (100 mg, 0.39 mmol) in DCM (8 mL) was cooled to 0° C. Diisobutylaluminium hydride (1 M in cyclohexane, 1.2 mL, 1.2 mmol) was added dropwise over 10 min. Then the mixture was stirred at 0° C. for 1 h. 2 mL of saturated ammonium chloride aqueous solution was added slowly to quench the reaction. Then 5 mL of saturated sodium bicarbonate aqueous solution was added. The mixture was extracted with DCM (3×10 mL). The combined organic layers were dried over sodium sulfate, filtered, and concentrated to give the crude product. The crude product was purified by column chromatography to give 42 mg of the product as a yellow solid. MS (ESI) m/z 214.1 [M+H]+.

WORKUP

后处理

  1. customto quench
  2. customthe reaction
  3. extractionThe mixture was extracted with DCM (3×10 mL)
  4. dry with materialThe combined organic layers were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto give the crude product
  8. customThe crude product was purified by column chromatography