Reaktion #215692

Reaktionsgleichung

n-Butyl glycolate

imidazole

t-butyldimethylchlorosilane

→

n-Butyl (t-butyl-dimethyl-silanyloxy)-acetate

Lösungsmittel

ether n-hexane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeare placed together at 0° C
2. 2
   SonstigeThe suspension obtained
3. 3
   Filtrationfiltered
4. 4
   WaschenThe crystals were rinsed thoroughly with ether/n-hexane 1:1 (200 ml)
5. 5
   WaschenThe filtrate was washed in succession with water (2×700 ml) and saturated aqueous sodium chloride solution (500 ml)
6. 6
   Trocknendried over magnesium sulphate
7. 7
   Einengenconcentrated
8. 8
   SonstigeThe oil obtained
9. 9
   workup.DISTILLATIONwas distilled over a Vigreux column (7.5 cm)

Vorschrift

n-Butyl glycolate (231 g; 1.75 mol) and imidazole (345.1 g; 5.07 mol) are placed together at 0° C. The suspension obtained was treated portionwise with t-butyldimethylchlorosilane (303 g; 2.01 mol) during 1.5 hours. After 20 hours at room temperature the reaction mixture was diluted with ether/n-hexane 1:1 (1 l) and suction filtered. The crystals were rinsed thoroughly with ether/n-hexane 1:1 (200 ml). The filtrate was washed in succession with water (2×700 ml) and saturated aqueous sodium chloride solution (500 ml), dried over magnesium sulphate and concentrated. The oil obtained was distilled over a Vigreux column (7.5 cm). Yield: 405 g (94%) as a colourless oil (b.p. 78° C./0.98 mmHg).

Quelle