Reaktion #554644

Reaktionsgleichung

cyclobutanol

5-bromo-2-chloro-pyrimidine

NaH

→

5-Bromo-2-cyclobutoxy-pyrimidine

Lösungsmittel

dioxane

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle