반응 #2122514

ord-203ce97f7b454c818798247fc1aa33a0

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 acetone (25 ml) until a gray colored solid
  3. 3
    기타separated
  4. 4
    기타The solid was collected by centrifugation
  5. 5
    세척washed with acetone
  6. 6
    기타dried under vacuum

실험 절차

A mixture of Compound 3 (1.0 g, 3.4 mmol) and p-toluenesulfonic acid methyl ester (0.94 g, 5.1 mmol) was heated in a pressure tube at 130° C. for 1 hour. The mixture was allowed to cool to room temperature, and the resulting mass was triturated with acetone (25 ml) until a gray colored solid separated. The solid was collected by centrifugation, washed with acetone and dried under vacuum to yield 1.4 g (86%) of Compound 4 whose structure is given below:

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08574881B2uspto-grants-2013_11