反应详情

A three-neck round-bottomed flask was immersed in a dry ice/ethanol cooling bath and equipped with a dry ice/ethanol condenser. The system was flushed with nitrogen and ammonia (approximately 50 mL) was condensed into the flask. (2R)-2-[[2-Amino-5-(benzylthio)[1,3]thiazolo[4,5-d]pyrimidin-7-yl](methyl)amino]-4-methylpentan-1-ol (1 g, 2.5 mmol) was added to the flask, resulting in a clear yellow solution. Small pieces of sodium metal (size 2-3 mm) were added one by one to the reaction mixture. When a persistent blue colour (>20 sec) appeared, a spoon of solid NH4Cl was added to quench the reaction. The ammonia was evaporated off. Water (50 mL) was added and the mixture was neutralized with 1M HCl (aq.) to pH 7. The precipitated yellow solid was collected by filtration, washed with water and dried in vacuo to yield 630 mg of the title compound (80% yield).

1. customA three-neck round-bottomed flask was immersed in a dry ice/ethanol cooling bath
2. customequipped with a dry ice/ethanol condenser
3. customThe system was flushed with nitrogen and ammonia (approximately 50 mL)
4. customcondensed into the flask
5. customresulting in a clear yellow solution
6. customa persistent blue colour (>20 sec)
7. customto quench
8. customthe reaction
9. customThe ammonia was evaporated off
10. additionWater (50 mL) was added
11. filtrationThe precipitated yellow solid was collected by filtration
12. washwashed with water
13. customdried in vacuo