HRID378790

反应详情

EQUATION

反应方程式

HRID 378790 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To methyl 4-azido-6-bromo-3-methoxypyridine-2-carboxylate (0.500 g, 1.74 mmol) in 10 mL of methanol was added NaBH4 (0.046 g, 1.22 mmol). The reaction mixture was stirred at room temperature for 10 min. Ethyl acetate and water were added and the phases were separated. The organic phase was washed with H2O, dried (MgSO4) and concentrated to dryness in vacuo. The residue was purified by chromatography (silica gel). Elution with 100% ethyl acetate gave 0.300 g of a white solid. 1H NMR(CDCl3): δ 3.90 (s, 1H); 3.95 (s, 1H); 4.60 (s, 2H); 6.85 (s, 1H).

WORKUP

后处理

  1. customthe phases were separated
  2. washThe organic phase was washed with H2O
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated to dryness in vacuo
  5. customThe residue was purified by chromatography (silica gel)
  6. washElution with 100% ethyl acetate