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Hexanoyl chloride → 4-Hexanamidophthalonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexanoyl chloride | HCID 67340 | — |
| 反応物 | 1,2-Benzenedicarbonitrile, 4-amino- | HCID 92529 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Hexanamidophthalonitrile | HCID 18466372 | 71% |
反応手順
4-Aminophthalonitrile (3.60 g, 25.2 2.mmole) was dissolved in 8.6 mL of pyridine. Hexanoyl chloride (8.6 10, 61.5 mmole) was added and the mixture was stirred under N2 for 2 hours. The pyridine was distilled under vacuum until a yellow-orange residue was obtained. This residue was dissolved in dichloromethane and washed with 0.1 M HCl (5×15 mL) and then neutralized with aqueous sodium bicarbonate (3×50 mL). The organic solution was separated and dried over magnesium sulfate. Purification by column chromatography (silica, dichloromethane: methanol 5%) afforded 4.3 g (71% yield) of 4-hexanamidophthalonitrile as a light yellow compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06274729B1 |
| 出典データセット | uspto-grants-2001_08 |
| ORD ID | ord-e3b80cb6e1b840558b6345b543a20676 |
| 出典メモ | uspto-grants-2001_08 |