反応 #214872

反応方程式

2,3-dihydrofuran

5-fluorouracil

p-toluenesulfonic acid

2,3-dihydrofuran

→

1-(2-tetrahydrofuryl)-5-fluorouracil

溶媒

pyridine

pyridine

反応条件

後処理

1. 1
   その他the mixture was reacted for 6 hours at 120° C. in an oil bath
2. 2
   その他the mixture was reacted for 15 hours
3. 3
   その他was removed from the reaction liquid by distillation
4. 4
   workup.DISSOLUTIONthe residue was dissolved in 100 ml of chloroform
5. 5
   ろ過filtered
6. 6
   その他to separate insoluble matters
7. 7
   洗浄The filtrate was washed with water
8. 8
   その他dried
9. 9
   濃縮concentrated
10. 10
    その他by removing chloroform
11. 11
    workup.DISTILLATIONby distillation
12. 12
    ろ過The precipitated crystals were collected by filtration
13. 13
    洗浄washed with a small amount of ether
14. 14
    その他dried

実験手順

In 50 ml of pyridine were dissolved 2.5 g of 5-fluorouracil and 0.4 g of p-toluenesulfonic acid. To this solution were added 1.5 ml of 2,3-dihydrofuran and the mixture was reacted for 6 hours at 120° C. in an oil bath. Further, 3 ml of 2,3-dihydrofuran in 4 portions were added and the mixture was reacted for 15 hours. After completion of the reaction, pyridine was removed from the reaction liquid by distillation and the residue was dissolved in 100 ml of chloroform and filtered to separate insoluble matters. The filtrate was washed with water, dried and concentrated by removing chloroform by distillation. The precipitated crystals were collected by filtration, washed with a small amount of ether and dried to obtain 2.0 g of 1-(2-tetrahydrofuryl)-5-fluorouracil. The crystals had a melting point of 167°-168° C. and were identical in IR-absorption spectra with the standard sample.

出典