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o-Butyl-aniline → (1-{6-[1-(2-Butyl-phenylimino)-ethyl]-pyridin-2-yl}-ethylidene)-(2,6-dimethyl-phenyl)-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | o-Butyl-aniline | HCID 75909 | — |
| 反応物 | 1-{6-[(1E)-N-(2,6-Dimethylphenyl)ethanimidoyl]pyridin-2-yl}ethan-1-one | HCID 22065624 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (1-{6-[1-(2-Butyl-phenylimino)-ethyl]-pyridin-2-yl}-ethylidene)-(2,6-dimethyl-phenyl)-amine | HCID 86674616 | — |
反応手順
1-{6-[1-(2,6-Dimethyl-phenylimino)-ethyl]-pyridin-2-yl}ethanone 1 (2.3 g, 0.0088 mol), 1.68 g (0.0244 mol) of 2-n-Butyl-phenylamine 12, 100 g of fresh molecular sieves, and 100 ml of toluene were kept at 100° C. for 3 days under the flow of nitrogen. The solvent was removed in a rotary evaporator and the residue was recrystallized from 5 ml of ethanol. The yield of (1-{6-[1-(2-n-butyl-phenylimino)-ethyl]-pyridin-2-yl}-ethylidene)-(2,6-dimethyl-phenyl)-amine 11 was 2.60 g (76%) as a yellow solid. 13C NMR (500 MHz, CD2Cl2, TMS (selected signals)): δ 166.8 (C═N), 166.1 (C═N).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08916664B2 |
| 出典データセット | uspto-grants-2014_12 |
| ORD ID | ord-9830a7de995e4cbeb2d685c30dc5545f |
| 出典メモ | uspto-grants-2014_12 |