반응 #87940

반응 방정식

4-[2,5-dioxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4,5,6,7,8-octahydro-quinazolin-4-yl]-3-methanesulfonyl-benzonitrile

INTERMEDIATE 18

4-[2,5-dioxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4,5,6,7,8-octahydro-quinazolin-4-yl]-3-methanesulfonyl-benzonitrile

cesium carbonate

2-bromoethylacetate

→

Acetic acid 2-[4-(4-cyano-2-methanesulfonyl-phenyl)-2,5-dioxo-1-(3-trifluoromethyl-phenyl)-1,4,5,6,7,8-hexahydro-2H-quinazolin-3-yl]-ethyl ester

용매

DMF

반응 조건

후처리

1. 1
   기타The mixture is purified by reversed phase HPLC (Waters SunFire™-C18, gradient of acetonitrile in water, 0.1% TFA)
2. 2
   기타1.07 min (Z018_S04)

실험 절차

To a solution of 4-[2,5-dioxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4,5,6,7,8-octahydro-quinazolin-4-yl]-3-methanesulfonyl-benzonitrile (INTERMEDIATE 18, 200 mg, 0.41 mmol) in DMF (4 mL) is added cesium carbonate (266 mg, 0.82 mmol) and 2-bromoethylacetate (91.0 μL, 0.82 mmol) and the mixture is stirred at 60° C. for 3 days. The mixture is purified by reversed phase HPLC (Waters SunFire™-C18, gradient of acetonitrile in water, 0.1% TFA). Yield: 60.0 mg; ESI mass spectrum [M+H]+=576; Retention time HPLC: 1.07 min (Z018_S04).

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