Reaktion #431284

Reaktionsgleichung

4'-[(2-n-butyl-benzimidazol-1-yl)-methyl]-2-(1-triphenylmethyl-tetrazol-5-yl)-biphenyl

hydrochloric acid

→

4'-[(2-n-Butyl-benzimidazol-1-yl)-methyl]-2-(1H-tetrazol-5-yl)-biphenyl

Lösungsmittel

methylene chloride

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe mixture is rotary evaporated to dryness in vacuum
2. 2
   workup.DISSOLUTIONThe residue is dissolved in methanol
3. 3
   Sonstigerotary evaporated once again
4. 4
   SonstigeThe crude product is purified over a silica gel column (grain size: 0.063-0.2 mm, eluting agent: methylene chloride/ethanol/ammonia=19:1:0.1)
5. 5
   SonstigeThe product is crystallised from ether
6. 6
   Sonstigedried at 50° C. in vacuum

Vorschrift

2 g (3 mmol) of 4'-[(2-n-butyl-benzimidazol-1-yl)-methyl]-2-(1-triphenylmethyl-tetrazol-5-yl)-biphenyl are dissolved in a mixture of 10 ml of methylene chloride and 10 ml of methanol, treated with 10 ml of etherified hydrochloric acid and stirred at ambient temperature for 3 hours. The mixture is rotary evaporated to dryness in vacuum. The residue is dissolved in methanol, rendered alkaline using ammonia and rotary evaporated once again. The crude product is purified over a silica gel column (grain size: 0.063-0.2 mm, eluting agent: methylene chloride/ethanol/ammonia=19:1:0.1). The product is crystallised from ether and dried at 50° C. in vacuum.

Quelle