HRID538430

反应详情

EQUATION

反应方程式

HRID 538430 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 2-nitro-3-methoxypyridine (32 g, 208 mmol) in EtOAc (150 mL) and MeOH (35 mL) under a nitrogen atmosphere was added 10% palladium on carbon (1.5 g, 1.4 mmol). This mixture was purged with H2 three times and the mixture was stirred for 3 h under a hydrogen atmosphere. The reaction mixture was purged with N2 three times, filtered through Celite, and the filter cake was washed with EtOAc (2×35 ml). The combined filtrate were concentrated and dried over high vacuum to afford 25.8 grams (100%) of 2-amino-3-methoxypyridine: LCMS (m/z): 125.0 (MH+); 1H NMR (300 MHz, CDCl3): 7.66 (m, 1H), 6.90 (m, 1H), 6.61 (m, 2H), 4.64 (s, br, 2H), 3.83 (s, 3H).

WORKUP

后处理

  1. customThis mixture was purged with H2 three times
  2. customThe reaction mixture was purged with N2 three times
  3. filtrationfiltered through Celite
  4. washthe filter cake was washed with EtOAc (2×35 ml)
  5. concentrationThe combined filtrate were concentrated
  6. customdried over high vacuum