تفاعل #1144437

معادلة التفاعل

chloromethyl ethyl ether

5-iodouracil

bistrimethylsilylacetamide

→

1-(ethoxy-methyl)-5-iodouracil

المردود 91.7%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   أخرىto form a homogeneous solution
2. 2
   درجة الحرارةheated
3. 3
   درجة الحرارةunder reflux for 3 hours
4. 4
   أخرىAfter the solvent was evaporated under reduced pressure
5. 5
   workup.ADDITIONthe residue was added with water
6. 6
   أخرىto produce crystals, which
7. 7
   ترشيحwere taken by filtration
8. 8
   غسيلThe crystals were washed
9. 9
   أخرىrecovering them
10. 10
    درجة الحرارةby cooling
11. 11
    ترشيحfiltration

الإجراء التجريبي

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.

المصدر