反応 #1144437

反応方程式

chloromethyl ethyl ether

5-iodouracil

bistrimethylsilylacetamide

→

1-(ethoxy-methyl)-5-iodouracil

収率 91.7%

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他to form a homogeneous solution
2. 2
   温度heated
3. 3
   温度under reflux for 3 hours
4. 4
   その他After the solvent was evaporated under reduced pressure
5. 5
   workup.ADDITIONthe residue was added with water
6. 6
   その他to produce crystals, which
7. 7
   ろ過were taken by filtration
8. 8
   洗浄The crystals were washed
9. 9
   その他recovering them
10. 10
    温度by cooling
11. 11
    ろ過filtration

実験手順

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.

出典