반응 #308609

반응 방정식

3-tert-butoxycarbonylamino-4-(2,4,5-trifluoro-phenyl)-butyric acid

triethylamine

3-trifluoromethyl-5,6,7,8-tetrahydro-imidazo[1,5-a]pyrazine

→

title compound

(R)-[3-oxo-1-(2,4,5-trifluoro-benzyl)-3-(3-trifluoromethyl-5,6-dihydro-8H-imidazo[1,5-a]pyrazin-7-yl)-propyl]-carbamic acid tert-butyl ester

용매

dichloromethane

반응 조건

후처리

1. 1
   workup.STIRRINGAfter stirring at room temperature for 5 minutes
2. 2
   기타The reaction mixture was reacted at room temperature for 2 hours
3. 3
   농축concentrated under reduced pressure
4. 4
   기타The resulting residue was purified by silica gel column chromatography

실험 절차

Under a nitrogen atmosphere, 3-tert-butoxycarbonylamino-4-(2,4,5-trifluoro-phenyl)-butyric acid 1k (8.6 g, 45 mmol) and 9.4 mL of triethylamine were dissolved in 300 mL of dichloromethane under stirring. After stirring at room temperature for 5 minutes, 3-trifluoromethyl-5,6,7,8-tetrahydro-imidazo[1,5-a]pyrazine if (15.0 g, 45 mmol) and bis(2-oxo-3-oxazolidinyl)phosphonic chloride (17.1 g, 67.3 mmol) were added to the solution successively. The reaction mixture was reacted at room temperature for 2 hours and monitored by thin layer chromatography until the disappearance of the starting materials and then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography to obtain the title compound (R-[3-oxo-1-(2,4,5-trifluoro-benzyl)-3-(3-trifluoromethyl-5,6-dihydro-8H-imidazo[1,5-a]pyrazin-7-yl)-propyl]carbamic acid tert-butyl ester 1l (20.0 g, yield 88%) as a white solid.

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