HRID79613

反应详情

EQUATION

反应方程式

HRID 79613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-bromo-4-fluoro-3-nitro-1H-pyrrolo[2,3-b]pyridine (2.0 g, 7.7 mmol) was placed in 6M HCl (30 mL) at room temperature. SnCl2 (7.29 g, 38.5 mmol) was then added, and the reaction was stirred for 30 minutes at room temperature. The reaction was then cooled to 0° C. and a saturated aqueous solution of Na2CO3 was added to raise the pH to 8. The reaction was then extracted with DCM (with minimal MeOH to aid solubility). The combined organic fractions were dried, filtered, and concentrated to give the crude product 5-bromo-4-fluoro-1H-pyrrolo[2,3-b]pyridin-3-amine (0.50 g, 28.2% yield), which was used without purification.

WORKUP

后处理

  1. temperatureThe reaction was then cooled to 0° C.
  2. temperatureto raise the pH to 8
  3. extractionThe reaction was then extracted with DCM (with minimal MeOH to aid solubility)
  4. customThe combined organic fractions were dried
  5. filtrationfiltered
  6. concentrationconcentrated