반응 #304530

ord-846af28f5f1b415eb694d2642f3d8dc3

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONThe reaction mixture were poured into ice-cold aqueous Na2CO3 solution
  2. 2
    추출extracted with ethyl acetate
  3. 3
    세척The organic layer washed with brine
  4. 4
    건조dried over anhydrous Na2SO4
  5. 5
    여과filtered
  6. 6
    농축concentrated in vacuo

실험 절차

A mixture of NaN3 (481 mg, 7.4 mmol) and 5-[1-chloro-2,2,2-trifluoro-eth-(Z)-ylideneamino]-4′-methyl-biphenyl-3-carboxylic acid methyl ester (1.3 g, 3.7 mmol) in 10 ml of dry ACN was stirred at room temperature for 16 hours. The reaction mixture were poured into ice-cold aqueous Na2CO3 solution, extracted with ethyl acetate. The organic layer washed with brine, dried over anhydrous Na2SO4, filtered, and concentrated in vacuo. The resulting crude 4′-methyl-5-(5-trifluoromethyl-tetrazol-1-yl)-biphenyl-3-carboxylic acid methyl ester (1.34 g, 99% yield) was used directly in the next step.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08193368B2uspto-grants-2012_06