반응 #90845

ord-39b0c928b5bb4aaa8ab300375efd17b3

반응 조건

온도
-20°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타drying (
  2. 2
    workup.ADDITIONa mixture of tert-butanol/water (50/50 v/v) as solvent),
  3. 3
    기타rotary evaporation
  4. 4
    기타quenching the melt
  5. 5
    기타The most suitable method, quenching the melt
  6. 6
    기타was selected for the preparation of the amorphous material
  7. 7
    온도the temperature was maintained for 10 minutes
  8. 8
    기타The samples were quenched in air
  9. 9
    기타to obtain an amorphous glass
  10. 10
    기타was determined at ca. 29° C. by modulated differential scanning calorimetry (MDSC)

실험 절차

Attempts were made to prepare amorphous tromethamine salt of bimatoprost acid by freeze drying (using a mixture of tert-butanol/water (50/50 v/v) as solvent), rotary evaporation and quenching the melt. The most suitable method, quenching the melt, was selected for the preparation of the amorphous material, followed by characterization before using this material as input material for the polymorphism study. In an attempt, Tromethamine Salt of Bimatoprost acid was heated in a vacuum oven at 120° C., the temperature was maintained for 10 minutes to melt the product. The samples were quenched in air and then cooled to −20° C. (freezer) to obtain an amorphous glass. The glass transition (Tg) was determined at ca. 29° C. by modulated differential scanning calorimetry (MDSC).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09447014B2uspto-grants-2016_09