HRID869712
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A suspension of ethyl 5,7-dihydroxypyrazolo[1,5-a]pyrimidine-2-carboxylate (9.59 g, 43.0 mmol) and phosphorous oxychloride (20.0 mL, 215 mmol) was refluxed for 1 hr. After being cooled to ambient temperature, the reaction mixture was poured into saturated sodium bicarbonate and chloroform. The organic layer was separated and aqueous layer was extracted with chloroform. The organic layer was combined and concentrated in vacuo to give ethyl 5,7-dichloropyrazolo[1,5-a]pyrimidine-2-carboxylate. MS (APCI): m/z 260/262 (M+H).
WORKUP
后处理
- temperaturewas refluxed for 1 hr
- customThe organic layer was separated
- extractionaqueous layer was extracted with chloroform
- concentrationconcentrated in vacuo