반응 #595325

반응 방정식

3,5,6-trifluoro-N1-(2-fluoro-4-iodophenyl)benzene-1,2-diamine

sulfonyl chloride

1-allyl-cyclopropanesulfonyl chloride

→

1-Allyl-cyclopropanesulfonic acid [3,4,6-trifluoro-2-(2-fluoro-4-iodo-phenylamino)phenyl]-amide

용매

pyridine

반응 조건

후처리

1. 1
   기타The reaction mixture was partitioned with water and EtOAc
2. 2
   세척The organic layer was washed with brine
3. 3
   기타dried (MGSO4)
4. 4
   농축concentrated under reduced pressure
5. 5
   기타The residue was purified by flash column chromatography on silica

실험 절차

To a stirred solution of the amine, i.e., 3,5,6-trifluoro-N1-(2-fluoro-4-iodophenyl)benzene-1,2-diamine, (1 eq) in anhydrous pyridine (5 ml/mmole) was added the sulfonyl chloride, i.e., 1-allyl-cyclopropanesulfonyl chloride, (1-5 eq). The reaction mixture was stirred at 40° C. for 48 hours. The reaction mixture was partitioned with water and EtOAc. The organic layer was washed with brine, dried (MGSO4) and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica. 1H NMR (CDCl3, 300 MHz): δ 7.41 (dd, 1H), 7.38 (dd, 1H), 7.09 (s, 1H), 6.78 (m, 1H), 6.49 (m, 1H), 5.96 (s, 1H), 5.86 (m, 1H), 5.18 (d, 2H), 2.76 (d, 2H), 1.23 (m, 2H), 0.872 (m, 2H).

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