반응 #2076927

ord-ca22774bae5c47c8a35e7094c9809c28

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed with 5% citric acid, sat. NaHCO3-sol
  2. 2
    기타Removal of the solvent in vacuum
  3. 3
    workup.WAITleft a crude product, which
  4. 4
    기타was purified by silica gel column chromatography with EtOAc

실험 절차

The title compound was prepared from 3-[6′-methyl-4′-(4-trifluoromethyl-phenyl)-[2,2′]bipyridinyl-6-yl]-benzenesulfonyl chloride (example I.2) (0.200 g, 0.409 mmol) by treatment with commercially available 2-(2-methoxy-ethoxy)-ethylamine [CAS-no. 31576-51-9] (0.244 mg, 2.04 mmol) in THF (5 mL) at 23° C. for 16 h. Diluted with EtOAc, washed with 5% citric acid, sat. NaHCO3-sol. and brine, dried organic layer over Na2SO4. Removal of the solvent in vacuum left a crude product, which was purified by silica gel column chromatography with EtOAc followed by trituration with diethyl ether/heptane to give the title compound (0.160 g, 68%) as a light yellow oil. MS (ISP) 572.2 [(M+H)+].

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07642264B2uspto-grants-2010_01