반응 #5977

ord-30b84fcc575343ca86cb76a38a32799d

반응 조건

온도
220°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타purified
  2. 2
    기타by dry column chromatography
  3. 3
    기타Three fractions are separated

실험 절차

A mixture of 0.6 g of methyl 2-(cyclohexen-3-yloxy)-4-acetylamino-5-chlorobenzoate and 0.5 ml diethylamiline is placed under house vacuum and heated to 220° C. for 2 hours. This reaction mixture is then diluted with 40% ethyl acetate/hexane and purified by dry column chromatography using the same solvent system as eluent. Three fractions are separated: 1. diethylaniline; 2. starting benzoate compound; and 3. methyl 3-(3-cyclohexenyl)-4-acetylamino-5-chlorosalicylate. The latter is used directly in the next step.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05246942uspto-grants-1993_09