반응 #1144437

반응 방정식

chloromethyl ethyl ether

5-iodouracil

bistrimethylsilylacetamide

→

1-(ethoxy-methyl)-5-iodouracil

수율 91.7%

용매

dichloromethane

반응 조건

후처리

1. 1
   기타to form a homogeneous solution
2. 2
   온도heated
3. 3
   온도under reflux for 3 hours
4. 4
   기타After the solvent was evaporated under reduced pressure
5. 5
   workup.ADDITIONthe residue was added with water
6. 6
   기타to produce crystals, which
7. 7
   여과were taken by filtration
8. 8
   세척The crystals were washed
9. 9
   기타recovering them
10. 10
    온도by cooling
11. 11
    여과filtration

실험 절차

In 50 ml of dichloromethane, 4.76 g (20 mmol) of 5-iodouracil was suspended and added with 11 ml (45 mmol) of bistrimethylsilylacetamide and stirred for 15 minutes at room temperature to form a homogeneous solution. This solution was added with 2.04 ml (22 mmol) of chloromethyl ethyl ether and 60 mg of tetra-n-butylammonium iodide and heated under reflux for 3 hours. After the solvent was evaporated under reduced pressure, the residue was added with water to produce crystals, which were taken by filtration. The crystals were washed by suspending them in hot methanol and recovering them by cooling and filtration to obtain 5.43 g of 1-(ethoxy-methyl)-5-iodouracil.

출처