HRID1426087

反应详情

EQUATION

反应方程式

HRID 1426087 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 250 mL round-bottomed flask was charged 3-(benzyloxy)-N-(4-methylthiazol-2-yl)pyridin-2-amine (11.4 g, 38.3 mmol) in 6M HCl (100 mL), and the reaction mixture was heated to reflux for 10 hours. The reaction mixture was cooled to room temperature, poured onto ice and saturated sodium bicarbonate, filtered, dried under vacuum and triturated with hexanes to afford 2-(4-methylthiazol-2-ylamino)pyridin-3-ol (6.23 g, 78.5% yield) as a pale yellow solid. 1H NMR (CD3OD) δ 7.79 (dd, 1H), 7.07 (dd, 1H), 6.79 (dd, 1H), 6.46 (q, 1H), 2.28 (s, 3H). LCMS (5 to 95) Rt=2.69 min (apci) m/z=208 (M+H).

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux for 10 hours
  3. filtrationfiltered
  4. customdried under vacuum
  5. customtriturated with hexanes