Reaktion #1583867

Reaktionsgleichung

dimethyl 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate

NaOH

→

title product

Ausbeute 57.2%

5-methoxycarbonyl-2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3-carboxylic acid

Ausbeute 57.2%

Lösungsmittel

methanol

methanol

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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%.

Quelle