Réaction #685001

ord-38c5ff8065e8407995cc02e55155403b

Équation de réaction

O=C(O)C(=O)O
oxalic acid
NC1CCN(CCOCCc2ccc3sccc3c2)C1
1-(2-(2-(1-benzothiophene-5-yl)ethoxy)ethyl)-3-pyrrolidinamine
NC1CCN(CCOCCc2ccc3sccc3c2)C1.O=C(O)C(=O)O.O=C(O)C(=O)O
achromatic crystal
Rendement 89.6%
NC1CCN(CCOCCc2ccc3sccc3c2)C1.O=C(O)C(=O)O.O=C(O)C(=O)O
1-(2-(2-(1-benzothiophene-5-yl)ethoxy)ethyl)-3-pyrrolidinamine dioxalate
Rendement 89.6%

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.ADDITIONwas added to the obtained solution
  2. 2
    workup.WAITat 5° C. for 1 hour
  3. 3
    AutreThereafter, precipitated crystals
  4. 4
    Filtrationwere collected by filtration
  5. 5
    Lavagewashed with ethyl acetate
  6. 6
    Autredried

Mode opératoire

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07897594B2uspto-grants-2011_03