Reaktion #685001
ord-38c5ff8065e8407995cc02e55155403b
Reaktionsgleichung
oxalic acid
1-(2-(2-(1-benzothiophene-5-yl)ethoxy)ethyl)-3-pyrrolidinamine
→
achromatic crystal
Ausbeute 89.6%
1-(2-(2-(1-benzothiophene-5-yl)ethoxy)ethyl)-3-pyrrolidinamine dioxalate
Ausbeute 89.6%
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONwas added to the obtained solution
- 2workup.WAITat 5° C. for 1 hour
- 3SonstigeThereafter, precipitated crystals
- 4Filtrationwere collected by filtration
- 5Waschenwashed with ethyl acetate
- 6Sonstigedried
Vorschrift
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.