반응 #1195752

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5-Amino-2-(4-methyl-3-oxopiperazin-1-yl)fluorobenzene

N,N-Dimethylaniline

benzyl chloroformate

→

5-benzyloxycarbonylamino-2-(4-methyl-3-oxopiperazin-1-yl)fluorobenzene

용매

DMF

ethyl acetate

반응 조건

후처리

1. 1
   workup.WAITto ambient over 16 hours
2. 2
   세척washed twice with water
3. 3
   기타After drying
4. 4
   기타(MgSO4) and evaporation of solvent
5. 5
   기타the residue was chromatographed on silica
6. 6
   온도a gradient increasing in polarity from 0 to 5% methanol in dichloromethane
7. 7
   기타evaporated

실험 절차

5-Amino-2-(4-methyl-3-oxopiperazin-1-yl)fluorobenzene (2.94 g) was dissolved in dry DMF (40 ml) under argon, and the solution cooled to -20° C. N,N-Dimethylaniline (2.1 ml) was added, followed by benzyl chloroformate (2.07 ml), and the mixture stirred for 10 minutes at -20° C. The temperature was allowed to rise to ambient over 16 hours. The mixture was diluted with ethyl acetate, and washed twice with water, and then brine. After drying (MgSO4) and evaporation of solvent, the residue was chromatographed on silica, using as eluant a gradient increasing in polarity from 0 to 5% methanol in dichloromethane. Relevant fractions were combined and evaporated to give 5-benzyloxycarbonylamino-2-(4-methyl-3-oxopiperazin-1-yl)fluorobenzene (4.6 g).

출처