تفاعل #671427

معادلة التفاعل

(2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(3,4-dimethylbenzyl)-4-[4-((3S)-3-methoxymethylmorpholino)-2-butynyl]piperazine

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(2R)-1-[3,5-bis-(trifluoromethyl)benzoyl]-2-(3,4-dimethylbenzyl)-4-[4-((3S)-3-methoxymethylmorpholino)butyl]piperazine

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   أخرىpalladium-carbon was removed by filtration
2. 2
   أخرىthe filtrate was evaporated under reduced pressure
3. 3
   أخرىThe residue was purified by column chromatography on silica gel with a mixture of methanol and ethyl acetate as an eluent

الإجراء التجريبي

A solution of (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(3,4-dimethylbenzyl)-4-[4-((3S)-3-methoxymethylmorpholino)-2-butynyl]piperazine (0.09 g) in methanol (10 ml) was hydrogenated in the presence of 10% palladium-carbon (40 mg) at room temperature. After 1 hour, palladium-carbon was removed by filtration and the filtrate was evaporated under reduced pressure. The residue was purified by column chromatography on silica gel with a mixture of methanol and ethyl acetate as an eluent to give (2R)-1-[3,5-bis-(trifluoromethyl)benzoyl]-2-(3,4-dimethylbenzyl)-4-[4-((3S)-3-methoxymethylmorpholino)butyl]piperazine. It was dissolved in ethyl acetate (10 ml) and 4N hydrogen chloride in ethyl acetate (0.5 ml) was added thereto. The mixture was evaporated in vacuo and the residue was triturated with a mixture of ethyl acetate and isopropyl ether to give (2R)-1-[3,5-bis(trifluoromethyl)benzoyl]-2-(3,4-dimethylbenzyl)-4-[4-((3S)-3-methoxymethylmorpholino)butyl]piperazine dihydrochloride (0.03 g) as a solid.

المصدر