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
- 52.5 °C
PROCEDURE
实验过程
A mixture of 1-propyl-8-(1H-pyrazol-4-yl)-3,7-bis-(2-trimethylsilanyl-ethoxymethyl)-3,7-dihydro-purine-2,6-dione (prepared as per literature procedure US20080194593) (0.1 g, 0.18 mmol), 1-(3-bromo-prop-1-ynyl)-4-methyl-benzene (prepared according to example E1) (0.039 g, 0.18 mmol), potassium carbonate (0.051 g, 0.37 mmol), and acetone (10 ml) were heated at 50-55° C. for 16 hours. Reaction mixture was cooled to 20-25° C. and filtered off. The filtrate was evaporated and residue was purified by preparative TLC to afford 1-propyl-8-[1-(3-p-tolyl-prop-2-ynyl)-1H-pyrazol-4-yl]-3,7-bis-(2-trimethylsilanyl-ethoxymethyl)-3,7-dihydro-purine-2,6-dione (0.035 g, 28%) as a brown sticky mass.
WORKUP
后处理
- customReaction mixture
- temperaturewas cooled to 20-25° C.
- filtrationfiltered off
- customThe filtrate was evaporated
- customresidue was purified by preparative TLC