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HRID 359863作成日:2026年10月25日

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

https://huagongshe.com/reaction/359863

反応式

関与物質

役割名称HCID仕込み量
反応物MethanolHCID 887—
反応物Sodium DithioniteHCID 24489—
反応物Sodium BicarbonateHCID 516892—
反応物1-methyl-3-{N-[[beta-[3,4-bis(isobutyryloxy)phenyl]ethyl]]carbamoyl}-pyridinium trifluoroacetateHCID 14050431—
溶媒WaterHCID 962—
溶媒Diethyl EtherHCID 3283—
生成物1-Methyl-3-{N-[[beta-[3,4-bis(isobutyryloxy)phenyl]ethyl]]carbamoyl}-1,4-dihydropyridineHCID 14050430—

反応手順

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: ##STR70##

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05002935
出典データセットuspto-grants-1991_03
ORD IDord-00b797e4a5a442b58458bc78d391a315
出典メモuspto-grants-1991_03