반응 #11764

ord-9080e5381cc74e3c8ad204cd6fbe546f

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed with water, 5% aqueous sodium hydrogen carbonate, and brine
  2. 2
    기타The organic layer was separated
  3. 3
    건조dried over sodium sulfate
  4. 4
    여과filtered
  5. 5
    농축concentrated in vacuo

실험 절차

To a solution of cesium carbonate (0.55 g, 1.70 mmol) in dimethylformamide (13 mL) was added thioacetic acid (0.24 g, 3.14 mmol) followed by addition of 4-chloro-2-chloromethyl-1-methoxybenzene (0.50 g, 2.62 mmol) in one portion. The reaction was stirred in the dark at ambient temperature overnight. The reaction was diluted with ethyl acetate, washed with water, 5% aqueous sodium hydrogen carbonate, and brine. The organic layer was separated, dried over sodium sulfate, filtered and concentrated in vacuo. Chromatography on silica gel gave the title compound (0.58 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07098212B2uspto-grants-2006_08