Reaction #64685

ord-14a88a091db240c3ae7f0ae0f07a0afd

Conditions

Temperature
90°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Otherprepared
  2. 2
    Temperaturemaintained at 90° C. for 2 hours
  3. 3
    workup.ADDITIONwere added to the reaction mixture
  4. 4
    Otherat 5° C.
  5. 5
    Otherfor 16 hours
  6. 6
    FiltrationAfter filtration the precipitate
  7. 7
    Washwas washed 3 times on the
  8. 8
    Filtrationfilter
  9. 9
    Otherdried at 40° C. under reduced pressure

Procedure

After weighing 14.4 g (0.1 mol) of Meldrum's acid and 16.6 g (0.1 mol) of veratraldehyde to 50 ml of the mixture of formic acid and triethylamine prepared according to Example 1, the reaction mixture was heated to 90° C. during 1 hour and maintained at 90° C. for 2 hours. After cooling down to room temperature 200 ml of ice-water were added to the reaction mixture, the pH value was adjusted to 1 by adding concentrated hydrochloric acid and the mixture was let stand at 5° C. for 16 hours. After filtration the precipitate was washed 3 times on the filter and dried at 40° C. under reduced pressure.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05414108uspto-grants-1995_05