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2,5-Difluoronitrobenzene → 2-(4-Fluoro-2-nitro-phenylamino)-5-isopropyl-benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,5-Difluoronitrobenzene | HCID 67767 | — |
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | 2-Amino-5-isopropylbenzonitrile | HCID 21093463 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 2-(4-Fluoro-2-nitro-phenylamino)-5-isopropyl-benzonitrile | HCID 21093459 | 81% |
反応手順
Heat a solution of 2-amino-5-isopropyl-benzonitrile (1.482 g, 9.25 mmol) with 1,4-difluoro-2-nitro-benzene (1.47 g, 9.25 mmol) and lithium hydroxide monohydrate (0.78 g, 18.50 mmol) in DMSO (20 ml) to 70° C. for 38 hours. Cool the reaction to ambient temperature and pour into approximately 200 ml of ice water and stir for one hour. Collect by filtration the title compound which precipitates. No further purification is necessary to obtain 2.236 g (7.47 mmol, 81% yield) of the title compound as an orange amorphous solid: Mass Spectrum (m/e): 300(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-6582b858a7dc4b12a586e38b3ad3f56b |
| 出典メモ | uspto-grants-2008_06 |