반응 #63084

반응 방정식

2-[2-(2,2,2-trifluoroethyl)guanidino]-4-(4-phthalimidobutyl)-5-methylthiazole hydrochloride

sodium hydroxide

hydrochloric acid

→

2-[2-(2,2,2-trifluoroethyl)guanidino]-4-(4-aminobutyl)-5-methylthiazole dihydrochloride

수율 128.6%

용매

water

ethanol

반응 조건

후처리

1. 1
   온도The resulting yellow solution was heated on a steam bath for 10 minutes
2. 2
   온도After cooling to ambient temperature the mixture
3. 3
   추출was extracted three times with equal volumes of ethyl acetate
4. 4
   기타The aqueous layer was evaporated to dryness
5. 5
   기타azeotroped twice with toluene
6. 6
   workup.DISSOLUTIONthe residue dissolved in methanol (10 ml.)
7. 7
   여과the solution filtered
8. 8
   기타The filtrate was evaporated to dryness

실험 절차

To a mixture of 2-[2-(2,2,2-trifluoroethyl)guanidino]-4-(4-phthalimidobutyl)-5-methylthiazole hydrochloride (0.60 g.) in water (2 ml.) and ethanol (2 ml.) was added sodium hydroxide pellets (0.2 g.). The resulting yellow solution was heated on a steam bath for 10 minutes and then allowed to cool to ambient temperature. The reaction mixture was adjusted to pH3 by addition of 2N hydrochloric acid and then reheated on a steam bath for 1 hour. After cooling to ambient temperature the mixture was extracted three times with equal volumes of ethyl acetate. The aqueous layer was evaporated to dryness, azeotroped twice with toluene, the residue dissolved in methanol (10 ml.) and the solution filtered. The filtrate was evaporated to dryness to give 2-[2-(2,2,2-trifluoroethyl)guanidino]-4-(4-aminobutyl)-5-methylthiazole dihydrochloride (0.31 g.) as an oil which was used without further purification.

출처