反应详情

温度

60 °C

20 g of sodium hydroxide (0.5 mol) are dissolved in 500 ml of ethanol/water at 1:1. 63.5 g of 4-amino-6-mercaptopyrimidine (0.5 mol) are added to the solution and the temperature of the solution is brought to 60° C. 115 g of p-toluene sulphonate of β-methoxyethyl (0.5 mol) are added drop by drop over 30 minutes, maintaining the temperature at 60° C. with a water bath. The addition terminated, the reaction mixture is refluxed for three hours. Then the solvent is evaporated and the residue is recovered with 250 ml of water. The aqueous solution is repeatedly extracted with chloroform (6×100 ml) and the amalgamated extracts are evaporated until dry. The solid residue is crystallised from ethyl acetate plus petroleum ether. 74 g of product are obtained (80% yield) with a melting point of 78°-80° C.

1. customis brought to 60° C
2. additionThe addition
3. customterminated
4. temperaturethe reaction mixture is refluxed for three hours
5. customThen the solvent is evaporated
6. customthe residue is recovered with 250 ml of water
7. extractionThe aqueous solution is repeatedly extracted with chloroform (6×100 ml)
8. customthe amalgamated extracts are evaporated
9. customuntil dry
10. customThe solid residue is crystallised from ethyl acetate plus petroleum ether