反応 #595325

反応方程式

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

溶媒

pyridine

反応条件

後処理

1. 1
   その他The reaction mixture was partitioned with water and EtOAc
2. 2
   洗浄The organic layer was washed with brine
3. 3
   その他dried (MGSO4)
4. 4
   濃縮concentrated under reduced pressure
5. 5
   その他The residue was purified by flash column chromatography on silica

実験手順

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).

出典