反応 #214876

ord-f67849dff878420f9ebbdb848aa04a0c

反応方程式

O=c1[nH]cc(F)c(=O)[nH]1
5-fluorouracil
C1=COCC1
2,3-dihydrofuran
O=c1[nH]c(=O)n(C2CCCO2)cc1F
1-(2-tetrahydrofuryl)-5-fluorouracil
収率 69.0%

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled
  2. 2
    その他was removed from the reaction liquid by distillation and 500 ml of chloroform and 5 g of silica gel
  3. 3
    workup.ADDITIONwere added to the residue
  4. 4
    ろ過filtered
  5. 5
    濃縮the filtrate was concentrated

実験手順

In 40 ml of pyridine were dissolved 5.2 g of 5-fluorouracil. The solution was ice cooled and 0.8 g of titanium tetrachloride was added thereto. Then, 6 ml of 2,3-dihydrofuran in 20 ml of pyridine were added to the mixture in 1.5 hours while stirring it at 80° C. The reaction was continued for 4 hours. After completion of the reaction, pyridine was removed from the reaction liquid by distillation and 500 ml of chloroform and 5 g of silica gel were added to the residue. The mixture was decolored and filtered and the filtrate was concentrated to obtain 5.5 g of 1-(2-tetrahydrofuryl)-5-fluorouracil in a yield of 69%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04256885uspto-grants-1981_03