Réaction #554644

Équation de réaction

cyclobutanol

5-bromo-2-chloro-pyrimidine

NaH

→

5-Bromo-2-cyclobutoxy-pyrimidine

Solvants

dioxane

Conditions de réaction

Traitement

1. 1
   AutreAfter removing of the cooling bath the reaction mixture
2. 2
   AutreThe reaction is quenched by the addition of water and sat. aq. NaHCO3 solution
3. 3
   AutreThe dioxane is removed in vacuo
4. 4
   Extractionthe aq. residue is extracted with DCM
5. 5
   Lavagewashed with water
6. 6
   Séchagedried with MgSO4
7. 7
   Filtrationfiltered
8. 8
   AutreThe solvent is removed under reduced pressure
9. 9
   AutreThe crude product is used without further purification

Mode opératoire

2.42 mL (31.0 mmol) cyclobutanol and 3.00 g (15.5 mmol) 5-bromo-2-chloro-pyrimidine are added to 40 mL dioxane and cooled down to 0° C. Then the reaction mixture is charged with 1.86 g (46.5 mmol) NaH. After removing of the cooling bath the reaction mixture is stirred at r.t. for 1 h. The reaction is quenched by the addition of water and sat. aq. NaHCO3 solution. The dioxane is removed in vacuo and the aq. residue is extracted with DCM. The org. phases are combined, washed with water, dried with MgSO4 and filtered. The solvent is removed under reduced pressure. The crude product is used without further purification.

Source