HRID1423315
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
- 115 °C
PROCEDURE
实验过程
A mixture of 6-oxo-1,4-dithiaspiro[4.4]nonane-7-carbonitrile (485 mg, 2.27 mmol) and 4-(6-phenylpyridin-3-yl)-1H-pyrazol-5-amine (537 mg, 2.27 mmol) in toluene (10 mL) was heated at 115° C. overnight. Concentration afforded crude 3-(6-phenylpyridin-3-yl)-6,7-dihydrospiro[cyclopenta[d]pyrazolo[1,5-a]pyrimidine-5,2′-[1,3]dithiolan]-8-amine, which was converted to 8-amino-3-(6-phenylpyridin-3-yl)-6,7-dihydro-5H-cyclopenta[d]pyrazolo[1,5-a]pyrimidin-5-one applying Stork's procedure (G. Stork, K. Zhao, Tetrahedron Letter, 1989, 30, 287) by treating with PhI(OCF3)2. LCMS tR=1.07 Min (5 min run, UV254nm), Mass calculated for, M+341.1, observed LC/MS m/z 342.1 (M+H).
WORKUP
后处理
- concentrationConcentration