반응 #790889

반응 방정식

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

용매

water

ether

ethyl ether

반응 조건

후처리

1. 1
   기타The ether layer was separated
2. 2
   추출the aqueous layer was extracted twice with ether
3. 3
   세척The combined ether extracts were washed with water
4. 4
   건조dried over sodium sulfate
5. 5
   기타Ether was removed under vacuum
6. 6
   기타leaving an oily product

실험 절차

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 had the structural formula: ##STR69##

출처