関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Chloroaniline | HCID 7812 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Boron Trichloride | HCID 25135 | — |
| 反応物 | 2,5-Dichlorobenzonitrile | HCID 89000 | — |
| 反応物 | Gallium monochloride | HCID 186022 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | (2-Amino-5-chlorophenyl)(2,5-dichlorophenyl)methanone | HCID 64422569 | — |
反応手順
To 28 ml of a 1M solution of trichloroborane at −5° C. are added 5.6 g of 4-chloroaniline dissolved in 30 ml of 1,2-dichloroethane. After 45 minutes at +15° C., 3.8 g of 2,5-dichlorobenzonitrile and 5 g of gallium trichloride are introduced and the mixture is refluxed for 3 hours. At room temperature, the resulting mixture is hydrolysed with 2M hydrochloric acid solution and maintained at 80° C. for 2 hours. The reaction medium is taken up in ethyl acetate and washed with water. The organic phase is dried over anhydrous sodium sulfate and concentrated. The residue is chromatographed on a column of silica gel, eluting with a cyclohexane/dichloromethane gradient to give 6.38 g of the expected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07396958B2 |
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| 出典データセット | uspto-grants-2008_07 |
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| ORD ID | ord-3778420d222746b59b371cebcda9fedb |
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| 出典メモ | uspto-grants-2008_07 |
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