Reaktion #157416

Reaktionsgleichung

HCl

1,4-dioxane

tert-butyl 4-(4-methoxyphenylcarbamoyl)-3-((pyridin-3-ylamino)methyl)piperazine-1-carboxylate TFA salt

→

title compound

Ausbeute 82.0%

N-(4-methoxyphenyl)-2-((pyridin-3-ylamino)methyl)piperazine-1-carboxamide dihydrochloride

Ausbeute 82.0%

Lösungsmittel

MeOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenthe reaction mixture was concentrated under reduced pressure
2. 2
   Sonstigepurified by HPLC (5 to 50% MeCN/0.1% TFA in H2O/0.1% TFA gradient)
3. 3
   workup.ADDITIONThe fractions containing the desired product
4. 4
   Einengenwere concentrated under reduced pressure
5. 5
   workup.DISSOLUTIONThe material was dissolved in MeOH (1 mL)
6. 6
   workup.ADDITIONtreated with 4 M HCl in 1,4-dioxane (6 mL)
7. 7
   EinengenThe mixture was concentrated under reduced pressure

Vorschrift

4 M HCl in 1,4-dioxane (6 mL, 24 mmol) was added to a solution of tert-butyl 4-(4-methoxyphenylcarbamoyl)-3-((pyridin-3-ylamino)methyl)piperazine-1-carboxylate TFA salt (81.7 mg, 0.147 mmol) in MeOH (1 mL). After 1 h, the reaction mixture was concentrated under reduced pressure and purified by HPLC (5 to 50% MeCN/0.1% TFA in H2O/0.1% TFA gradient). The fractions containing the desired product were concentrated under reduced pressure. The material was dissolved in MeOH (1 mL) and treated with 4 M HCl in 1,4-dioxane (6 mL). The mixture was concentrated under reduced pressure to give 49.9 mg (82%) of the title compound as a white solid. LC-MS: RT=1.95 min, [M+H]+=342.1.

Quelle