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HRID 5652作成日:2026年10月23日

Hydrochloric Acid → 5-Carboxy-2-methylthiomethyl-6-methyl-4-(3-nitrophenyl)-3-carboethoxy-1,4-dihydropyridine

https://huagongshe.com/ja/reaction/5652

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrochloric AcidHCID 313—
反応物TriphenylphosphineHCID 11776—
反応物Ammonium formateHCID 2723923—
反応物2-Methylthiomethyl-6-methyl-4-(3-nitrophenyl)-3-carboethoxy-5-carboallyloxy-1,4-dihydropyridineHCID 19796419—
触媒PalladiumHCID 23938—
溶媒1,4-DioxaneHCID 31275—
生成物5-Carboxy-2-methylthiomethyl-6-methyl-4-(3-nitrophenyl)-3-carboethoxy-1,4-dihydropyridineHCID 19796518—

反応手順

A suspension of 2-methylthiomethyl-6-methyl-4-(3-nitrophenyl)-3-carboethoxy-5-carboallyloxy-1,4-dihydropyridine (g 0.27), palladium on charcoal (10% 6 mg), ammonium formate (mg 71) and triphenylphosphine (mg 3) in anhydrous 1,4-dioxane, is heated at the reflux temperature for 8 hours. The reaction mixture is cooled at room temperature, poured into an aqueous solution of hydrochloric acid (pH=2) and extracted with ethyl acetate (2×20 ml). The combined organic extracts are washed with aqueous sodium carbonate (1N; 3×10 l), the basic washings are collected, acidified to pH 5-6 with diluted aqueous hydrochloric acid. The resulting suspension is extracted with ethyl acetate (2×25 ml) the combined organic extracts are dried on Na2SO4 and evaporated under reduced pressure to give mg 160 of 5-carboxy-2-methylthiomethyl-6-methyl-4-(3-nitrophenyl)-3-carboethoxy-1,4-dihydropyridine as an amorphous solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05245039
出典データセットuspto-grants-1993_09
ORD IDord-6c49a90aeb7b4f16adbda904ec4ca422
出典メモuspto-grants-1993_09