HRID2041927
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
- 47.5 °C
PROCEDURE
实验过程
In a 250 mL pressure tube, Hg(OAc)2 (2.52 g, 7.88 mmol) was suspended in vinyl acetate (73 mL, 788 mmol). To this suspension was added H2SO4/EtOAc (1.5 mL/15 mL). A clear solution was formed. The 2-iodo-6-chloro-9H-purine (22.1 g, 78.8 mmol) was added. A suspension formed again. It was degassed and stirred at 45-50° C. overnight. A dark solution was formed. The mixture was passed through celite, washed with EtOAc. Organic layer was washed with Sat. NaHCO3, dried Na2SO4. The product was purified on silica gel chromatography column (1-5% MeOH/DCM).
WORKUP
后处理
- customA clear solution was formed
- customA suspension formed again
- customIt was degassed
- customA dark solution was formed
- washwashed with EtOAc
- washOrganic layer was washed with Sat. NaHCO3, dried Na2SO4
- customThe product was purified on silica gel chromatography column (1-5% MeOH/DCM)