Réaction #1583867

ord-60c066ce929e440abb6a308e530d6fa5

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrewas conducted at 70° C.
  2. 2
    workup.STIRRINGunder violent stirring for 6 hours
  3. 3
    Autreevaporated under reduced pressure
  4. 4
    Autreto remove 80 mL methanol
  5. 5
    workup.ADDITIONTo the residue was added 200 mL water
  6. 6
    AutreThe unreacted starting materials are removed by filtration
  7. 7
    Autreto separate a yellow solid, which
  8. 8
    Filtrationwas filtered
  9. 9
    Autredried
  10. 10
    Autreto produce a khaki powder

Mode opératoire

3.5 g dimethyl 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate (0.01 mol) and 150 mL methanol were mixed. To the mixture was added a saturated aqueous NaOH solution (9 g, 0.225 mol) under stirring. The reaction was conducted at 70° C. under violent stirring for 6 hours, and evaporated under reduced pressure to remove 80 mL methanol. To the residue was added 200 mL water. The unreacted starting materials are removed by filtration. The filtrate was adjusted to a pH of about 2.5 with 1 mol/L hydrochloric acid to separate a yellow solid, which was filtered and dried to produce a khaki powder. The resulting powder was treated with methanol to produce the title product as a yellow solid (1.9 g) in a yield of 57.2%.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US09198902B2uspto-grants-2015_12