反応 #2275686

反応方程式

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

HCl

dioxane

2,2-dimethoxypropane

→

liquid

収率 100.0%

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

収率 100.0%

溶媒

Triethylamine

DMAC

反応条件

後処理

1. 1
   その他the 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
   ろ過The mixture was filtered
5. 5
   洗浄the collected solid washed several times with ethyl acetate
6. 6
   その他The filtrate was then evaporated on a high vacuum rotary evaporator at 40° C.

実験手順

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).

出典