반응 #46235

ord-f2f858c7533640c5baeee336b83ab6da

용매

반응 조건

온도
75°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The volatiles were evaporated
  2. 2
    기타re-evaporated with chloroform-toluene
  3. 3
    workup.ADDITIONThe residual brown oil was diluted with chloroform (22 mL)

실험 절차

4-(6-(1-(Benzo[d][1,3]dioxol-5-yl)cyclopropanecarboxamido)pyridin-2-yl)benzenesulfonic acid (1.9 g, 4.3 mmol) was dissolved in POCl3 (30 mL) followed by the addition of SOCl2 (3 mL) and DMF (100 μl). The reaction mixture was heated at 70-80° C. for 15 min. The volatiles were evaporated and then re-evaporated with chloroform-toluene. The residual brown oil was diluted with chloroform (22 mL) and used for sulfonylation immediately. ESI-MS m/z calc. 456.0. found 457.1 (M+1).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07741321B2uspto-grants-2010_06