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Acetic Acid → 2-Mercaptomethyl-3,5-dicarboetoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Diethyl 2-(chloromethyl)-6-methyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate | HCID 3064723 | — |
| 反応物 | 1-Butanaminium,N,N,N-tributyl-, sulfide (1:1) | HCID 16205437 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Mercaptomethyl-3,5-dicarboetoxy-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine | HCID 11675833 | 70.4% |
反応手順
A solution of 2-chloromethyl-3,5-dicarboethoxy-4-(m-nitrophenyl) -6-methyl-1,4-dihydropyridine (1 g) and tetrabutylammonium hydrogen sulfide (0.7 g) in methylene chloride (10 ml) is stirred at -10° C. for 20 minutes, neutralized with a drop of AcOH, evaporated under vacuum and the residue recrystallized from Et2O to give 0.7 g of 2-mercaptomethyl-3,5-dicarboethoxy-4-(m-nitrophenyl)-6-methyl-1, 4-dihydropyridine, m.p. 145°-147° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04999362 |
| 出典データセット | uspto-grants-1991_03 |
| ORD ID | ord-7e14a53e5d704020aa01189f8f162012 |
| 出典メモ | uspto-grants-1991_03 |