반응 #1605995

ord-4455730859824dbcaf78ebbd4c4306cd

반응 조건

온도
90°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.DISSOLUTIONcompletely dissolved
  2. 2
    온도cooled
  3. 3
    농축concentrated
  4. 4
    workup.ADDITION10% methanol in dichloromethane was added
  5. 5
    여과the mixture was filtered

실험 절차

A mixture of EXAMPLE 173B (22.12 g), water (43 mL), and triethylamine (43.6 mL) in 1,4-dioxane (300 mL) was stirred at room temperature until EXAMPLE 173B completely dissolved. The solution was then treated with 4-chloro-3-nitrobenzenesulfonamide, heated at 90° C. for 16 hours, cooled and concentrated. 10% methanol in dichloromethane was added, and the solution was stirred vigorously at room temperature until a fine suspension existed and the mixture was filtered.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09072748B2uspto-grants-2015_07