반응 #2030121

ord-c15b1f7e076347e0bacd443ee7230ed3

반응 조건

온도
130°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to cool to room temperature
  2. 2
    기타the resulting mass was triturated with ethyl acetate (25 ml) until an off-white solid
  3. 3
    기타separated
  4. 4
    기타The solid was collected by centrifugation
  5. 5
    세척washed with ethyl acetate
  6. 6
    기타dried under vacuum

실험 절차

A mixture of Compound 24 (2.0 g, 7.8 mmol) and p-toluenesulfonic acid methyl ester (2.2 g, 11.7 mmol) was heated in a pressure tube at 130° C. for 2 hours. The mixture was allowed to cool to room temperature, and the resulting mass was triturated with ethyl acetate (25 ml) until an off-white solid separated. The solid was collected by centrifugation, washed with ethyl acetate and dried under vacuum to yield 2.9 g (84%) of Compound 25 whose structure is given below:

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08389729B2uspto-grants-2013_03