반응 #685001

반응 방정식

oxalic acid

1-(2-(2-(1-benzothiophene-5-yl)ethoxy)ethyl)-3-pyrrolidinamine

→

achromatic crystal

수율 89.6%

1-(2-(2-(1-benzothiophene-5-yl)ethoxy)ethyl)-3-pyrrolidinamine dioxalate

수율 89.6%

용매

ethyl acetate

ethyl acetate

반응 조건

후처리

1. 1
   workup.ADDITIONwas added to the obtained solution
2. 2
   workup.WAITat 5° C. for 1 hour
3. 3
   기타Thereafter, precipitated crystals
4. 4
   여과were collected by filtration
5. 5
   세척washed with ethyl acetate
6. 6
   기타dried

실험 절차

0.71 g of 1-(2-(2-(1-benzothiophene-5-yl)ethoxy)ethyl)-3-pyrrolidinamine was dissolved in 3.0 ml of ethyl acetate. Thereafter, 4.0 ml of an ethyl acetate solution containing 0.44 g of oxalic acid was added to the obtained solution, and the obtained mixture was stirred at a room temperature for 1 hour and then at 5° C. for 1 hour. Thereafter, precipitated crystals were collected by filtration, washed with ethyl acetate, and then dried, so as to obtain 1.03 g of an achromatic crystal, 1-(2-(2-(1-benzothiophene-5-yl)ethoxy)ethyl)-3-pyrrolidinamine dioxalate.

출처