반응 #5954

ord-7dae953e4f5249e8b8c29ff501f4aac0

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed for 16 h
  2. 2
    기타The solvent was evaporated
  3. 3
    여과filtered
  4. 4
    기타evaporated to dryness
  5. 5
    workup.ADDITIONwhich was treated with hydrogen chloride in ether

실험 절차

A mixture of 3,4,5-trimethoxyphenylisothiocyanate (2.0 mmol) (produced as in Example 22) and 3-[4-(2-chlorophenyl) -1-piperazinyl]propanol (510 mg; 2.0 mmol) in toluene (40 ml) was refluxed for 16 h. The solvent was evaporated and the residue resuspended in ethyl acetate filtered and evaporated to dryness. The residue was submitted to flash chromatography on silica gel 60 eluting with toluene/ethyl acetate (1:1). The product was taken up in ethanol, which was treated with hydrogen chloride in ether to give 220 mg of the title compound. M.p. 182°-183° C. MS (70 eV): m/z 479 (M+, 0.5%), 254 (47), 225 (82), 209 (100), 182 (29).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05246935uspto-grants-1993_09