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
PROCEDURE
实验过程
Br--AcO--HxR, 415 mg (1.0 mmol), was dissolved in 30 ml of methanol containing 0.24 ml of triethylamine and 170 mg of 10% palladium carbon was added to the solution. While stirring the mixture at room temperature, hydrogen gas was passed in a flow rate of 40 ml/min. After the palladium carbon was filtered off, the filtrate was washed with ethanol and the solvent was distilled off under reduced pressure. The residue was dissolved in 8 ml of methanol and 0.54 ml of 28% sodium methoxide (methanolic solution) was added to the solution. The mixture was stirred at room temperature for 30 minutes. The reaction solution was quantitatively determined by HPLC, where 63.7 mg (0.27 mmoles) of 2',3'-dideoxyinosine and 93.2 mg (0.37 mmoles) of 3'-deoxyinosine were produced in yields of 7% and 37%, respectively. 300 MHz nuclear magnetic resonance spectra of the purified and isolated 2',3'-dideoxyinosine and 3'-deoxyinosine supported the structures of the products.
WORKUP
后处理
- additionwas added to the solution
- filtrationAfter the palladium carbon was filtered off
- washthe filtrate was washed with ethanol
- distillationthe solvent was distilled off under reduced pressure
- dissolutionThe residue was dissolved in 8 ml of methanol
- addition0.54 ml of 28% sodium methoxide (methanolic solution) was added to the solution
- stirringThe mixture was stirred at room temperature for 30 minutes