Reaktion #988300

Reaktionsgleichung

product

8-Butyl-7-(3-(((1,1-dimethylethoxy)carbonyl)-imidazol-5-yl)-1-oxopropyl)-2-(2-methoxyphenyl)-5,6,7,8-tetrahydro-imidazo[1,2-a]pyrazine

HCl

→

product

Ausbeute 47.0%

8-Butyl-7-(3-(imidazol-5-yl)-1-oxopropyl)-2-(2-methoxyphenyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine

Ausbeute 47.0%

Lösungsmittel

MeOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeSolvents were removed under reduced pressure
2. 2
   Sonstigeto yield 420 mg of crude product
3. 3
   SonstigePart of the crude (100 mg) was purified by preparative HPLC on a RAININ™ C18 column (Varian Analytical, Walnut Creek, Calif.)
4. 4
   workup.WAITHCl (pH=2.0) over 45 minutes with UV detection at 254 nm
5. 5
   EinengenProduct fractions were concentrated to about ½ volume

Vorschrift

The product from Step 1.g. (450 mg, 0.89 mmol) was dissolved in MeOH (5 ml) and 4N HCl was added and the reaction was stirred at room temperature for about ½ hour. Solvents were removed under reduced pressure to yield 420 mg of crude product. Part of the crude (100 mg) was purified by preparative HPLC on a RAININ™ C18 column (Varian Analytical, Walnut Creek, Calif.) using a gradient of 10-30% CH3CN/aq. HCl (pH=2.0) over 45 minutes with UV detection at 254 nm. Product fractions were concentrated to about ½ volume and lyophilized to yield pure product (47 mg, 47%) as the di-hydrochloride. Mass spec. 508.2 MH−.

Quelle