HRID1250699

反应详情

EQUATION

反应方程式

HRID 1250699 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 1-(3-aminopropyl)-4-[2-pyridyl]pyridinium bromide hydrobromide (6 g, 16 mmol) in MeOH (150 mL) at 0° C. was added NaBH4 (2 g, 53 mmol) in small portions over a period of 2 h. The reaction mixture was stirred overnight at room temperature and the solvent was evaporated. The residue was suspended in ether (200 mL) and treated with 50% NaOH solution (100 mL). The ether layer was separated and the aqueous layer was extracted with ether (2×50 mL). The combined ether extracts were dried over potassium carbonate and the solvent was removed to give 3-(3′,6′-dihydro-2′-H-[2,4′]bipyridinyl-1′-yl)-propylamine as an oil. It was immediately used in the next step without purification.

WORKUP

后处理

  1. customthe solvent was evaporated
  2. additiontreated with 50% NaOH solution (100 mL)
  3. customThe ether layer was separated
  4. extractionthe aqueous layer was extracted with ether (2×50 mL)
  5. dry with materialThe combined ether extracts were dried over potassium carbonate
  6. customthe solvent was removed