HRID1177399
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
A mixture of ethyl 2-(2,6-dichloropyridin-3-ylamino)-2-thioxoacetate (49.11 g, 175.9 mmol) and cesium carbonate (57.32 g, 175.9 mmol) in THF (350 mL) was heated at 50° C. for 6 h. The reaction suspension was then diluted with water (700 mL) and THF was removed in vacuo at 23° C. The resulting suspension was cooled to 0° C., and the precipitated solid was collected via vacuum filtration, washed with water, and dried in vacuo to provide ethyl 5-chlorothiazolo[5,4-b]pyridine-2-carboxylate as a yellow-orange solid. MS (ESI) m/z: Calculated: 242.0; Observed: 243.0 (M++1).
WORKUP
后处理
- customwas removed in vacuo at 23° C
- temperatureThe resulting suspension was cooled to 0° C.
- filtrationthe precipitated solid was collected via vacuum filtration
- washwashed with water
- customdried in vacuo