반응 #57409

ord-cfb2860a59194e57b88e49052db281d3

용매

반응 조건

온도
28°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The flask is then cooled in an ice bath
  2. 2
    온도The reaction is then heated to 60° C.
  3. 3
    기타is obtained
  4. 4
    온도it is cooled to and
  5. 5
    온도maintained at room temperature
  6. 6
    기타to quench
  7. 7
    기타the reaction
  8. 8
    온도The resulting slurry is cooled in an ice bath
  9. 9
    여과filtered

실험 절차

α-Bromotricyclo[3.3.1.13,7]decane-1-acetic acid (Formula O) is then reacted with H2SO4 and HNO3 to produce α-bromo-3-hydroxytricyclo[3.3.1.13,7]decane-1-acetic acid (Formula Q). More specifically, α-bromo-3-hydroxytricyclo[3.3.1.13,7]decane-1-acetic acid (Formula Q) is prepared from α-bromotricyclo[3.3.1.13,7]decane-1-acetic acid (Formula O) by first charging an Erlen-Meyer flask with H2SO4. The flask is then cooled in an ice bath and 50% HNO3 is added to the flask. The solid α-bromotricyclo[3.3.1.13,7]decane-1-acetic acid (Formula O) is then added to the mixture in portions which maintain the temperature under 28° C. The reaction is then heated to 60° C. with stirring until a clear solution is obtained. When the reaction is complete, it is cooled to and maintained at room temperature. Water is then added to quench the reaction. The resulting slurry is cooled in an ice bath and then filtered to obtain α-bromo-3-hydroxytricyclo [3.3.1.13,7]decane-1-acetic acid (Formula Q). See also Example 18 herein.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07420079B2uspto-grants-2008_09