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-5-methylbenzonitrile | HCID 242778 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 5-Methyl-2-(2-nitro-phenylamino)-benzonitrile | HCID 21093537 | 57.1% |
反応手順
Combine 1-fluoro-2-nitro-benzene (4.34 g, 30.79 mmol), 2-amino-5-methyl-benzonitrile (4.07 g, 30.79 mmol), lithium hydroxide monohydrate (2.58 g, 61.58 mmol) and DMSO (50.0 ml). Stir the mixture at 55° C. for 22 hours, cool to ambient temperature and pour the mixture onto ice chips and stir. After 1 hour, remove the resulting precipitate by vacuum filtration. Dry the precipitate under vacuum, purify on silica gel using dichloromethane/hexanes (75:25) to give 4.45 g (57%) of an orange solid: mp 135-139° C.; 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 | US07384934B2 |
|---|
| 出典データセット | uspto-grants-2008_06 |
|---|
| ORD ID | ord-59a7b2194a9e4d2abdfafb97986af174 |
|---|
| 出典メモ | uspto-grants-2008_06 |
|---|