化工社化工社 化学情報印刷レポート · 研究参考用
Methylamine → N-Methyl-2,6-dinitroaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | 1-Chloro-2,6-dinitrobenzene | HCID 11814 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-Methyl-2,6-dinitroaniline | HCID 80010 | 91% |
反応手順
Methylamine (4.5 ml of 2.0 M solution in THF) was added to a stirred solution of 2-chloro-1,3-dinitrobenzene (0.90 g, 4.4 mmol) in 40 ml of THF and the mixture was stirred for 30 min. The reaction was quenched by the addition of water and ether. The aqueous layer was separated and extracted twice with ether. The combined organic extracts were washed with saturated NaHCO3, brine and dried over magnesium sulfate. Filtration, removal of solvent and purification of residue via Biotage chromatography eluting with 20% ethyl acetate/dichloromethane to gave 0.80 g (91%) of product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07714009B2 |
| 出典データセット | uspto-grants-2010_05 |
| ORD ID | ord-b3575c850ed24abfb186b9218c0bcd5c |
| 出典メモ | uspto-grants-2010_05 |