반응 #1121733

반응 방정식

water

3-(dimethylamino)-1,2-propanediol

imidazole

tert-butyldimethylsilyl chloride

→

1-(tert-butyldimethylsilyloxy)-3-(dimethylamino)propan-2-ol

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   기타The organic layer was separated
2. 2
   추출the aqueous layer was extracted with two additional portions of dichloromethane (20 mL)
3. 3
   건조The combined organic extracts were dried (MgSO4)
4. 4
   여과filtered
5. 5
   농축concentrated

실험 절차

A dry dichloromethane (10 mL) solution of 3-(dimethylamino)-1,2-propanediol (98%, 1.00 g, 8.39 mmol, 1.0 equiv) and imidazole (0.57 g, 8.39 mmol, 1.0 equiv) was stirred at 0° C. under argon for 15 minutes. Solid tert-butyldimethylsilyl chloride (1.26 g, 8.39 mmol, 1.0 equiv) was added to the mixture and the resultant was stirred for 2 hours at 0° C. The mixture was then diluted with 20 mL of dichloromethane and poured into deionized water (15 mL). The organic layer was separated and the aqueous layer was extracted with two additional portions of dichloromethane (20 mL). The combined organic extracts were dried (MgSO4), filtered and concentrated to afford crude 1-(tert-butyldimethylsilyloxy)-3-(dimethylamino)propan-2-ol, a thick clear oil, which was used without further purification.

출처