関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Ammonium formate | HCID 2723923 | — |
| 反応物 | 2-Methylthiomethyl-6-methyl-4-(3-nitrophenyl)-3-carboethoxy-5-carboallyloxy-1,4-dihydropyridine | HCID 19796419 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 5-Carboxy-2-methylthiomethyl-6-methyl-4-(3-nitrophenyl)-3-carboethoxy-1,4-dihydropyridine | HCID 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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05245039 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-6c49a90aeb7b4f16adbda904ec4ca422 |
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| 出典メモ | uspto-grants-1993_09 |
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