Réaction #2619

ord-6520b67c10374e1083985864bd8780e4

Équation de réaction

COc1ccccc1N(CCN1CCC(C(=O)c2ccc(F)cc2)CC1)C(=O)c1ccc(CNC(=O)[C@H](C)N)cc1
4-[(S)-2-Aminopropionyl]aminomethyl-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(2-methoxyphenyl)benzamide
O=C(O)C(=O)O
oxalic acid
COc1ccccc1N(CCN1CCC(C(=O)c2ccc(F)cc2)CC1)C(=O)c1ccc(CNC(=O)[C@H](C)N)cc1.O=C(O)C(=O)O.O=C(O)C(=O)O
title compound
Rendement 85.1%
COc1ccccc1N(CCN1CCC(C(=O)c2ccc(F)cc2)CC1)C(=O)c1ccc(CNC(=O)[C@H](C)N)cc1.O=C(O)C(=O)O.O=C(O)C(=O)O
4-[(S)-2-Aminopropionyl]aminomethyl-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(2-methoxyphenyl)benzamide dioxalate
Rendement 85.1%

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autremethanol was removed by evaporation
  2. 2
    Lavagethe resulting amorphous residue was washed with acetone (5 ml)
  3. 3
    Filtrationcollected by filtration

Mode opératoire

4-[(S)-2-Aminopropionyl]aminomethyl-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(2-methoxyphenyl)benzamide (84.7 mg, 0.155 mmol) was dissolved in methanol (5 ml) and mixed with oxalic acid (28 mg, 0.311 mmol). After 5 minutes of stirring at room temperature, methanol was removed by evaporation, and the resulting amorphous residue was washed with acetone (5 ml) and collected by filtration to obtain 84 mg (85.1%) of the title compound in a colorless amorphous powder form.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05728835uspto-grants-1998_03