تفاعل #6864

معادلة التفاعل

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

المردود 47.0%

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

المردود 47.0%

المذيبات

MeOH

ظروف التفاعل

المعالجة

1. 1
   أخرىSolvents were removed under reduced pressure
2. 2
   أخرىto yield 420 mg of crude product
3. 3
   أخرىPart 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
   تركيزProduct fractions were concentrated to about ½ volume

الإجراء التجريبي

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+.

المصدر