반응 #83624

반응 방정식

(-)(2aR,4S)-6-(3-isoxazolyl)-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indole

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title product

수율 14.2%

(-)(4R)-6-(3-isoxazolyl)-4-(di-n-propylamino)-1,3,4,5-tetrahydrobenz[cd]indole

수율 14.2%

용매

CH2Cl2

반응 조건

후처리

1. 1
   기타was sonicated at 50-55 KHz for four hours
2. 2
   온도The reaction mixture was warmed
3. 3
   온도to reflux during the time period
4. 4
   여과the reaction mixture was filtered through a celite pad
5. 5
   농축the filtrate was concentrated to dryness in vacuo
6. 6
   기타The resulting residue was chromatographed (flash column, silica gel, EtOAc)

실험 절차

A mixture of (-)(2aR,4S)-6-(3-isoxazolyl)-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indole (400 mg, 1.2 mmol) and 1 g of MnO2 in 100 ml of CH2Cl2 was sonicated at 50-55 KHz for four hours. The reaction mixture was warmed to reflux during the time period. After four hours, the reaction mixture was filtered through a celite pad and the filtrate was concentrated to dryness in vacuo. The resulting residue was chromatographed (flash column, silica gel, EtOAc) to provide 55 mg of title product as an oil. MS m/e 323 (FD)

출처