반응 #2275686

반응 방정식

N-(hydroxyethyl)-amino-2,3-propanediol

HCl

dioxane

2,2-dimethoxypropane

→

liquid

수율 100.0%

2-[(2,2-Dimethyl-[1,3]-dioxolan-4-yl-methyl)-amino]-ethanol

수율 100.0%

용매

Triethylamine

DMAC

반응 조건

후처리

1. 1
   기타the solvents removed by rotary evaporation
2. 2
   workup.DISSOLUTIONThe viscous crude mixture was dissolved into triethylamine (30 mL) and ethyl acetate (500 mL)
3. 3
   workup.STIRRINGstirred at RT for 30 min
4. 4
   여과The mixture was filtered
5. 5
   세척the collected solid washed several times with ethyl acetate
6. 6
   기타The filtrate was then evaporated on a high vacuum rotary evaporator at 40° C.

실험 절차

The N-(hydroxyethyl)-amino-2,3-propanediol (16.5 g, 122 mmol) was treated with a solution of HCl in dioxane (33.5 ml, 134 mmol). To this solution were added 2,2-dimethoxypropane (15.3 g, 147 mmol), DMAC (50 mL), and a catalytic amount of para-toluene sulphonic acid (0.006 mol, 1.16 g). The mixture stirred at room temperature for 24 hours. Triethylamine (1 mL) was then added, and the solvents removed by rotary evaporation. The viscous crude mixture was dissolved into triethylamine (30 mL) and ethyl acetate (500 mL) and stirred at RT for 30 min. The mixture was filtered and the collected solid washed several times with ethyl acetate. The filtrate was then evaporated on a high vacuum rotary evaporator at 40° C. to give a yellow liquid (0.122 mol, 99% yield).

출처