반응 #816434

ord-8cda38af14924b15933ff6035202f0db

용매

반응 조건

온도
150°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타It was evaporated
  2. 2
    추출the residue was extracted with DCM
  3. 3
    기타The organic layer was dried
  4. 4
    기타evaporated

실험 절차

Potassium tert-butoxide (0.309 g, 1.83 mmol) was added to a solution of N-ethyl-1-[4-(trifluoromethyl)phenyl]methanesulfonamide (0.49 g, 1.83 mmol) and diethyl oxalate (0.322 g, 2.20 mmol) in THF (4 mL) at 0° C. The mixture was heated in a microwave reactor at 150° C. for 10 mins. HCl (1M, 2 mL) was added dropwise to the mixture at 0° C. It was evaporated and the residue was extracted with DCM. The organic layer was dried and evaporated to give the title compound (0.480 g, 81%) as a solid; 1H NMR (500 MHz, CDCl3): δ 8.05 (d, 2H), 7.77 (d, 2H), 3.87 (q, 2H), 1.49 (t, 3H); Mass Spectrum: M−H+ 320.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07582629B2uspto-grants-2009_09