HRID448554

反应详情

EQUATION

反应方程式

HRID 448554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1H-pyrrolo[3,2-b]pyridine (1.18 g, 10 mmol) in 100 mL of THF, was added borane tetrahydrofuran complex (60 mL of a 1 M solution, 6 eq) and the mixture was heated at reflux for 5 h. After allowing the reaction to cool down to room temperature, water was added slowly and the solution was extracted with ethyl acetate twice. The combined extracts were washed with a saturated solution of sodium bicarbonate, dried over sodium sulfate and evaporated. The residue was purified on silica gel (eluent: 15% methanol in DCM) to give 0.17 g of 2,3-dihydro-1H-pyrrolo[3,2-b]pyridine 1-1.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 5 h
  3. customthe reaction
  4. extractionthe solution was extracted with ethyl acetate twice
  5. washThe combined extracts were washed with a saturated solution of sodium bicarbonate
  6. dry with materialdried over sodium sulfate
  7. customevaporated
  8. customThe residue was purified on silica gel (eluent: 15% methanol in DCM)