HRID2278991

反应详情

EQUATION

反应方程式

HRID 2278991 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of N-(6-methyl-5-((2-(3-methylisoxazol-5-yl)pyridin-4-yl)oxy)pyridin-2-yl)acetamide (0.11 g, 0.339 mmol) and 2M HCl (1.696 mL, 3.39 mmol) in THF (3 mL) was heated at 60° C. for 4 h. The mixture was cooled to RT, treated with EtOAc and H2O, neutralized with NaHCO3, the layers separated and the aqueous layer extracted with EtOAc (1×). The combined organics were washed with brine, dried over Na2SO4 and concentrated to dryness to afford 6-methyl-5-((2-(3-methylisoxazol-5-yl)pyridin-4-yl)oxy)pyridin-2-amine (90 mg, 94%) as a white solid. 1H NMR (400 MHz, DMSO-d6): δ 8.51 (d, J=5.7 Hz, 1 H); 7.26 (d, J=2.5 Hz, 1 H); 7.22 (d, J=8.7 Hz, 1 H); 6.95 (s, 1 H); 6.89 (dd, J=5.7, 2.5 Hz, 1 H); 6.36 (d, J=8.7 Hz, 1 H); 6.00 (s, 2 H); 2.28 (s, 3 H); 2.06 (s, 3 H); MS (ESI) m/z: 283.1 (M+H+).

WORKUP

后处理

  1. temperatureThe mixture was cooled to RT
  2. customthe layers separated
  3. extractionthe aqueous layer extracted with EtOAc (1×)
  4. washThe combined organics were washed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated to dryness