반응 #660394

반응 방정식

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

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate (2×300 mL)
2. 2
   세척After washing with water and brine
3. 3
   건조the organic layer was dried over Na2SO4
4. 4
   여과filtered

실험 절차

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.

출처