関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Fluoro-2-nitroaniline | HCID 67769 | — |
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | 2-Fluoro-5-(trifluoromethyl)benzonitrile | HCID 521016 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 2-(4-Fluoro-2-nitro-phenylamino)-5-trifluoromethyl-benzonitrile | HCID 21093461 | 96% |
反応手順
Combine 4-fluoro-2-nitro-phenylamine (5.0 g, 32.03 mmol), 2-fluoro-5-trifluoromethyl-benzonitrile (6.07 g, 32.03 mmol) and lithium hydroxide monohydrate (4.03 g, 96.08 mmol) in methyl sulfoxide (DMSO, 60 ml). Heat the resulting mixture to 70° C. for 16 hours. Cool the reaction mixture to ambient temperature, then pour into approximately 400 ml of ice water and stir for one hour. Filter the resulting mixture and collect the precipitate to obtain 9.995 g of the title compound (30.73 mmol, 96% yield) as an orange amorphous solid. Product used as is with no further purification: Mass Spectrum (m/e): 326(M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07384934B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-709a5f8e5dfe4658858302fdd37086d6 |
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| 出典メモ | uspto-grants-2008_06 |
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