Reaktion #1130415

Reaktionsgleichung

pyridine hydrofluoride

solution

1,5,8-trioxadispiro[2.2.2.4]dodecane

polyethylene

Na2CO3

→

crude product

(8-fluoro-1,4-dioxaspiro[4.5]decan-8-yl)methanol

Lösungsmittel

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with ethyl acetate (2×300 mL)
2. 2
   WaschenAfter washing with water and brine
3. 3
   Trocknenthe organic layer was dried over Na2SO4
4. 4
   Filtrationfiltered

Vorschrift

A solution of pyridine hydrofluoride (4 g) in dichloromethane (10 mL) was added dropwise to a solution of EXAMPLE 443A (1.7 g) in dichloromethane (20 mL) in a polyethylene bottle at 0° C. The mixture was stirred at room temperature overnight. The mixture was carefully poured over a mixture of ice-water and Na2CO3 and extracted with ethyl acetate (2×300 mL). After washing with water and brine, the organic layer was dried over Na2SO4, and filtered. Concentration of the filtrate gave the crude product.

Quelle