تفاعل #595325
ord-182caf2807d84ef799efe0560e10dc7d
معادلة التفاعل
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
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
40°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىThe reaction mixture was partitioned with water and EtOAc
- 2غسيلThe organic layer was washed with brine
- 3أخرىdried (MGSO4)
- 4تركيزconcentrated under reduced pressure
- 5أخرىThe residue was purified by flash column chromatography on silica
الإجراء التجريبي
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).