化工社化工社 化学情報印刷レポート · 研究参考用
Methylamine → N-Methyl-1-(methylsulfanyl)-2-nitroethan-1-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | 1,1-Bis(methylthio)-2-nitroethylene | HCID 83623 | — |
| 反応物 | 1,2-Dichloroethane ethanol | HCID 22901612 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | N-Methyl-1-(methylsulfanyl)-2-nitroethan-1-amine | HCID 15788612 | — |
反応手順
A solution of methylamine in ethanol/ethylenedichloride (112.5 ml of 33% ethanolic methylamine in 0.8 liters of ethylene dichloride; 0.94 mole) was added over 51/2 hr at 70° to a stirred solution of 1,1-bismethylthio-2-nitroethene (99.0 g, 0.6 mole) in ethylene dichloride (1.5 litres). The solution was heated to boiling and 0.7 liters of solvent were distilled off. The cooled solution was washed with 2 N hydrochloric acid (0.25 liters), then with brine (0.25 liters). The solvent was removed and the residue crystallised from isopropyl acetate (0.5 liters), treating the hot solution with charcoal (10.0 g). The product (35.0 g) formed yellow prisms, m.p. 114°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04169855 |
| 出典データセット | uspto-grants-1979_10 |
| ORD ID | ord-398c82f5d14c448492bab9c8b502c38c |
| 出典メモ | uspto-grants-1979_10 |