반응 #359922

반응 방정식

mixture

3-chloro-8-methoxy-11-oxo-10,11-dihydro-5H-dibenzo[b,e][1,4]diazepin-7-yl trifluoromethanesulfonate

1-vinyl-2-pyrrolidinone

triethylamine

→

title compound

3-chloro-8-methoxy-7-[1-(2-oxopyrrolidin-1-yl)vinyl]-5,10-dihydro-11H-dibenzo[b,e][1,4]diazepin-11-one

용매

DMF

ethyl acetate

반응 조건

후처리

1. 1
   세척washed with water and brine
2. 2
   건조dried (MgSO4)
3. 3
   여과filtered
4. 4
   농축concentrated
5. 5
   기타The concentrate was purified by column chromatography on silica gel using a solvent gradient that
6. 6
   온도increased from 1 to 4% methanol in dichloromethane

실험 절차

A mixture of Example 516A, 1-vinyl-2-pyrrolidinone, Pd(dppf)Cl2-CH2Cl2, and triethylamine in DMF was heated at 110° C. overnight, cooled to room temperature, diluted with ethyl acetate, washed with water and brine, dried (MgSO4), filtered and concentrated. The concentrate was purified by column chromatography on silica gel using a solvent gradient that increased from 1 to 4% methanol in dichloromethane to give the title compound. MS (ESI) m/e 384 (M+H)+.

출처