Реакция #4673

Уравнение реакции

1-methyl-3-{N-[[β-[3,4-bis(isobutyryloxy)phenyl]ethyl]]}carbamoylpyridinium trifluoroacetate

methanol

NaHCO3

sodium dithionite

→

1-Methyl-3-{N-[[β-[3,4-bis(isobutyryloxy)phenyl]ethyl]]}carbamoyl-1,4-dihydropyridine

Растворители

water

ether

ethyl ether

Условия реакции

Обработка

1. 1
   ДругоеThe ether layer was separated
2. 2
   Экстракцияthe aqueous layer was extracted twice with ether
3. 3
   ПромывкаThe combined ether extracts were washed with water
4. 4
   Сушкаdried over sodium sulfate
5. 5
   ДругоеEther was removed under vacuum
6. 6
   Другоеleaving an oily product

Методика

A solution of 0.55 g (1 mmol) of 1-methyl-3-{N-[[β-[3,4-bis(isobutyryloxy)phenyl]ethyl]]}carbamoylpyridinium trifluoroacetate in 50 ml of deaerated water containing 10 ml of methanol was extracted three times with 30 ml portions of ether. To the resultant aqueous solution were added NaHCO3 (0.25 g, 3 mmol) and 50 ml of ethyl ether and the mixture was kept under nitrogen. To this ice-cold mixture was added sodium dithionite (0.52 g, 3 mmol) and the mixture was stirred vigorously for 30 minutes. The ether layer was separated and the aqueous layer was extracted twice with ether. The combined ether extracts were washed with water and dried over sodium sulfate. Ether was removed under vacuum, leaving an oily product. NMR analysis confirmed that the product has the structural formula: ##STR39##

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