반응 #167759

ord-8654c9004bf5476abf41d465b9644743

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture was cooled to 0° C.
  2. 2
    여과the precipitates were collected by filtration

실험 절차

The compound 12 obtained at Step (2) (503 mg) was dissolved in acetonitrile (0.5 ml), p-toluenesulfonic acid monohydrate in an acetonitrile solution (0.69M, 2 ml) was added at 60° C., then the mixture was allowed to gradually cool to room temperature. After 3 hours, the mixture was cooled to 0° C. and further stirred for 1.5 hours, then the precipitates were collected by filtration to obtain the title compound (535 mg) as a colorless crystals.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846660B2uspto-grants-2014_09