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Sodium Hydroxide → HCID 19831143、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Fumaric Acid | HCID 444972 | — |
| 反応物 | 2-Bromoethylamine hydrobromide | HCID 2774217 | — |
| 反応物 | (-)-2-[(1,4,5,6-Tetrahydropyrimidin-2-yl)thio]methyl-3-carboethoxy-5-carbomethoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine | HCID 19796531 | — |
| 触媒 | Hexadecyltributylphosphonium bromide | HCID 84716 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 19831143 | HCID 19831143 | — |
反応手順
A mixture of (-)-2-[(1,4,5,6-tetrahydropyrimidin-2-yl)thio]methyl-3-carboethoxy-5-carbomethoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine (g 2), hexadecyltributyl phosphonium bromide (mg 180), 2-bromoethylaminehydrobromide (mg 900), NaOH (35%, ml 8) and benzene is stirred for 40 minutes at room temperature. After the usual work-up, an oily residue is obtained that is dissolved in ethyl acetate and treated with fumaric acid to give 1.9 g of (-)-2-(aminoethylthio)methyl-3-carboethoxy-5-carbomethoxy-4-(3-nitrophenyl)-6-methyl-1,4-dihydropyridine fumarate, m.p. 104°-110° C. [α]D =-11 (C=4 in MeOH).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05245039 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-7e2beb4a11a24e89994da680a2a56493 |
| 出典メモ | uspto-grants-1993_09 |