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Benzoyl chloride → HCID 178509345、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzoyl chloride | HCID 7412 | — |
| 反応物 | Trimethylsilyl cyanide | HCID 82115 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | 1-(4-Chloroanilino)phthalazine | HCID 22741997 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178509345 | HCID 178509345 | — |
反応手順
Under N2 atmosphere, first 164 mg (1.2 mmol) anhydrous aluminium chloride is added to 12.6 g (49.3 mmol) 1-(4-chloroanilino)phthalazine in 90 ml dichloromethane, followed by 12.3 ml (98.6 mmol) trimethylsilyl cyanide. Finally, 11.5 ml (98.6 mmol) benzoyl chloride is added under ice cooling and stirred for 3 h at RT. The suspension is poured onto 0.6 ml water, filtered off, washed with water, and dried. Mixing in 150 ml boiling ethanol yields pure title compound: m.p.: 201-202° C.; Anal. calc.(C22H15N4ClO) C, 68.31%; H, 3.91%; N, 14.48%, Cl, 9.16%; found C, 68.03%; H, 3.89%; N, 14.22%; Cl, 9.42%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06514974B2 |
| 出典データセット | uspto-grants-2003_02 |
| ORD ID | ord-e08578a0d938466aace99e1a6ef63031 |
| 出典メモ | uspto-grants-2003_02 |