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Oxalic Acid → N-Methyl-5-[[[2-[(1-methylthio-2-nitroethenyl) amino]ethyl]thio]methyl]-2-furanmethanamine, oxalate salt
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Oxalic Acid | HCID 971 | — |
| 反応物 | 1,1-Bis(methylsulfanyl)-2-nitroethane | HCID 12372264 | — |
| 反応物 | 5-[[(2-Aminoethyl)thio]methyl]-N-methyl-2-furanmethanamine | HCID 20209492 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-Methyl-5-[[[2-[(1-methylthio-2-nitroethenyl) amino]ethyl]thio]methyl]-2-furanmethanamine, oxalate salt | HCID 131711940 | 26.6% |
反応手順
A solution of 2-[[5-[(methylamino)methyl]-2-furanylmethyl]thio]ethanamine (6.0 g) and 1,1-bis-(methylthio)-2-nitroethane (19.8 g) in dry dimethylformamide (150 ml) was stirred for 1 hour at 0° and for 5 hours at room temperature. A solution of oxalic acid (4.0 g) in dry dimethylformamide (16 ml) was added and the solid which formed during 18 hours was filtered, washed with dimethylformamide, ethanol and ether and dried. The solid was suspended in water (200 ml) at 55° and on cooling was filtered, washed with water and dried to give the title compound (3.25 g) m.p. 158°-160° dec.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04233302 |
| 出典データセット | uspto-grants-1980_11 |
| ORD ID | ord-36f2bc0b14104a2596250c41c9eacbfe |
| 出典メモ | uspto-grants-1980_11 |