関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Fluoro-2-nitrobenzene | HCID 73895 | — |
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | 2-Amino-4-methylbenzonitrile | HCID 2801276 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 4-Methyl-2-(2-nitro-phenylamino)-benzonitrile | HCID 21093529 | — |
反応手順
Combine 1-fluoro-2-nitro-benzene (5.34 g, 37.83 mmol), 2-amino-4-methyl-benzonitrile (5.00 g, 37.83 mmol), lithium hydroxide monohydrate (3.17 g, 75.66 mmol) and DMSO (70.0 ml). Stir the mixture at 55° C. for 16 hours then cool it to ambient temperature. Pour the mixture onto ice chips and stir for 1 hour. Remove the resulting yellow precipitate by vacuum filtration. Dry the precipitate under vacuum then recrystallize it in ethanol to give 5.15 g (54%) of fine, amber colored needles: mp 162–164°; mass spectrum (ion spray): m/z=254.0 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07214673B2 |
|---|
| 出典データセット | uspto-grants-2007_05 |
|---|
| ORD ID | ord-b8f1c9b8df5b401d9c01e94183af269a |
|---|
| 出典メモ | uspto-grants-2007_05 |
|---|