Reaktion #334231

Reaktionsgleichung

2-hydroxyethyl isopropyl 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylate

nitric acid

sodium hydroxide

→

2-Hydroxyethyl isopropyl 2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylate

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   TemperaturThe mixture was then cooled down to 5° to 10° C.
3. 3
   SonstigeThe oil which had separated out
4. 4
   Extraktionwas extracted with methylene chloride
5. 5
   Trocknenthe extracts were dried over sodium sulphate
6. 6
   Sonstigeevaporated in vacuo
7. 7
   Sonstigeto crystallize by trituration with ether/petroleum ether
8. 8
   Filtrationfiltered off with suction
9. 9
   Sonstigerecrystallized from methanol

Vorschrift

20 g (49.5 mmol) of 2-hydroxyethyl isopropyl 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylate were introduced into a mixture of 83 ml of 96% strength nitric acid in 660 ml of water and heated to boiling for 1 hour. The mixture was then cooled down to 5° to 10° C. and made weakly alkaline with dilute sodium hydroxide solution. The oil which had separated out was extracted with methylene chloride, the extracts were dried over sodium sulphate and evaporated in vacuo. The oily residue was induced to crystallize by trituration with ether/petroleum ether, filtered off with suction and recrystallized from methanol.

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