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1-Fluoro-2-nitrobenzene → 4-Methyl-2-(2-nitro-phenylamino)-benzonitrile
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) and stir at 55° C. Afer 16 hours; cool to ambient temperature, pour the mixture onto ice chips and stir. After 1 hour, remove the resulting yellow precipitate by vacuum filtration. Dry the precipitate under vacuum, recrystallize in ethanol to give 5.15 g (54%) of fine, amber colored needles: mp 162-164° 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-357fcf9ce6314f65ad7576ea9c7b50b7 |
| 出典メモ | uspto-grants-2008_06 |