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Dimethylamine → Dimethyl-(3-nitrobenzyl)-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Benzene, 1-(bromomethyl)-3-nitro- | HCID 77568 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Dimethyl-(3-nitrobenzyl)-amine | HCID 308050 | — |
反応手順
A solution of 3-nitrobenzyl bromide (10, 1.67 g, 7.73 mmol) and N,N-dimethylamine (4.25 mL, 2M in THF) in anhydrous THF (30 mL) was heated at 40° C. overnight. The reaction mixture was diluted with 1N HCl (30 mL, aq.), the aqueous layer separated, and extracted with EtOAc (30 mL). The pH of the aqueous layer was then adjusted to 9 using saturated Na2CO3 (aq.) and the aqueous layer was extracted with EtOAc (50 mL). The organic layer was washed with water (40 mL), brine (40 mL), and dried over Na2SO4. The solids were filtered and the filtrate was concentrated on a rotavap to give 11 (1.2 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07265122B2 |
| 出典データセット | uspto-grants-2007_09 |
| ORD ID | ord-c7988076d0cf49a78bf5a45bf0b280d9 |
| 出典メモ | uspto-grants-2007_09 |