HRID889897

反应详情

EQUATION

反应方程式

HRID 889897 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 15.2 g (46.2 mmol) 2-(7-chloro-thieno[3,2-b]pyridin-2-yl)-4-methyl-thiazole-5-carboxylic acid ethyl ester, 80 mL of THF and 20 mL of absolute ethanol was added (13 g, 231 mmol) freshly ground potassium hydroxide. The reaction was stirred at room temperature for sixteen hours. The reaction was cooled to 0° C. and the pH was adjusted to pH 3 with conc HCl. The resulting yellow precipitate was filtered and dried to give 2-(7-chloro-thieno[3,2-b]pyridin-2-yl)-4-methyl-thiazole-5-carboxylic acid (10.3 g) in 72% yield. C12H7N2O2S2: APCI m/z 310.2/312.2 (pos.); 1H NMR (d6-DMSO): δ 8.67 (d, 1H, J=5.0 Hz), 8.42 (s, 1H), 7.65 (d, 1H, J=5.0 Hz), 2.65 (s, 3H) ppm.

WORKUP

后处理

  1. temperatureThe reaction was cooled to 0° C.
  2. filtrationThe resulting yellow precipitate was filtered
  3. customdried