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
The 5-Amino-1-β-ribofuranosylimidazole-4-carboxamide (1.3 g, 5 mmol) was dissolved in pyridine and 18 ml (15 mmol) phenyl-isothiocyanate were added slowly. The reaction mixture was refluxed for 2 hours under argon atmosphere. The solution was cooled to room temperature, the precipitate collected by filtration and washed with diethyl ether. The obtained pyridinium salt of the product was dissolved in aqueous sodium hydroxide (15%, 40 ml). The solution was heated 30 minutes at 60° C. and concentrated under vacuum. Methanol was then added and the solution was kept in the refrigerator overnight. After 20 hours the precipitated colourless prisms were collected by filtration to give 1.2 g (80%) 2-Mercaptoinosine.
WORKUP
后处理
- temperatureThe reaction mixture was refluxed for 2 hours under argon atmosphere
- filtrationthe precipitate collected by filtration
- washwashed with diethyl ether
- dissolutionThe obtained pyridinium salt of the product was dissolved in aqueous sodium hydroxide (15%, 40 ml)
- temperatureThe solution was heated 30 minutes at 60° C.
- concentrationconcentrated under vacuum
- additionMethanol was then added
- customwas kept in the refrigerator overnight
- filtrationAfter 20 hours the precipitated colourless prisms were collected by filtration