تفاعل #491469

ord-ea8a6a5ef39141ab8782760242eef892

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةgradually warmed up to room temperature
  2. 2
    workup.STIRRINGto stir for 18 hr
  3. 3
    تجفيفThe organic layer was dried over anhydrous Na2SO4
  4. 4
    أخرىevaporated
  5. 5
    أخرىto afford the crude product, which

الإجراء التجريبي

mCPBA (77%, 0.0550 g, 0.246 mmol) was added to N-(but-3-enyl)-2-nitro-N-phenylbenzenesulfonamide (0.0653 g, 0.196 mmol) in 1 mL CHCl3 at 0° C. The mixture was stirred at 0° C. for 30 min, then gradually warmed up to room temperature and continued to stir for 18 hr. After TLC showed the disappearance of starting material, the reaction mixture was diluted with a 1:1 mixture of water and saturated NaHCO3 (2×10 mL) and water (10 mL). The organic layer was dried over anhydrous Na2SO4 and evaporated to afford the crude product, which was subjected to silica gel chromatography using Hexanes/EtOAc to afford 0.0662 g colorless oil as product, yield 96.9%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08748473B2uspto-grants-2014_06