反应详情

To 2 ml of dimethyl sulfoxide, 468 mg (2.0 mmol) of 6-phenylthiothymine, 358 mg (1.0 mmol) of 4-(t-butyldimethylsiloxy)-butyl-p-toluenesulphonate and 276 mg (2.0 mmol) of potassium carbonate were added and heated to react for 4 hours at 80° C. The reaction mixture was concentrated under reduced pressure, added with methanol and filtered. The filtrate was concentrated under reduced pressure, added with 20 ml of tetrahydrofuran and 1 ml of 1N hydrochloric acid and stirred for 90 minutes. The reaction mixture was concentrated under reduced pressure and adsorbed on a silica gel column and eluted with 2% methanol/chloroform. The eluate was concentrated and crystallized from acetone/hexane to obtain 12.0 mg of the target compound (Yield: 4%).

1. temperatureheated
2. customto react for 4 hours at 80° C
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. additionadded with methanol
5. filtrationfiltered
6. concentrationThe filtrate was concentrated under reduced pressure
7. additionadded with 20 ml of tetrahydrofuran and 1 ml of 1N hydrochloric acid
8. concentrationThe reaction mixture was concentrated under reduced pressure
9. washeluted with 2% methanol/chloroform
10. concentrationThe eluate was concentrated
11. customcrystallized from acetone/hexane