Reaktion #1285024

Reaktionsgleichung

Methyl (±)-[5-[amino(4-fluorophenyl)methyl]-1H-benzimidazol-2-yl]carbamate

HCl

→

Methyl (±)-[5-[Amino(4Fluorophenyl)Methyl]-1H-Benzimidazol-2-yl]Carbamate Dihydrochloride Salt

Lösungsmittel

MeOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITat 5° C. for 18 hours
2. 2
   FiltrationThe solid was collected by filtration
3. 3
   SonstigeThe salt was recrystallized
4. 4
   workup.ADDITIONadding water (250 mL) until a solution
5. 5
   Sonstigewas obtained
6. 6
   FiltrationThe solution was filtered through a Celite pad
7. 7
   Sonstigeevaporated to dryness
8. 8
   Filtrationthen collected by filtration yield: 175 g (66%) of the title dihydrochloride, mp.>315° C.

Vorschrift

Methyl (±)-[5-[amino(4-fluorophenyl)methyl]-1H-benzimidazol-2-yl]carbamate (209 g, 0.67 mole) was suspended in 2.4 L of MeOH containing (1.5 m HCl) of 12N aq HCl and stirred at room temperature for 24 hours and then at 5° C. for 18 hours. The solid was collected by filtration. The salt was recrystallized by suspending the solid in MeOH (3 L) and adding water (250 mL) until a solution was obtained. The solution was filtered through a Celite pad and evaporated to dryness. The solid was again suspended in MeOH then collected by filtration yield: 175 g (66%) of the title dihydrochloride, mp.>315° C.

Quelle