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Dichloromethane → 5-Methyl-2-nitrobenzoyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 5-Methyl-2-nitrobenzoic acid | HCID 18371 | — |
| 反応物 | Phosphorus pentachloride | HCID 24819 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 5-Methyl-2-nitrobenzoyl chloride | HCID 3016013 | — |
反応手順
The reaction of 36.2 g of 5-methyl-2-nitrobenzoic acid and 41.6 g of phosphorus pentachloride in 150 ml of toluene gave a crude product which was treated with methylene chloride to give 5-methyl-2-nitrobenzoyl chloride as an oil. When 30 g of this acid chloride in 50 ml of tetrahydrofuran was added to a warm solution of 30.9 g of 5-aminotetrazole monohydrate in 600 ml of tetrahydrofuran and 30 ml of water, a precipitate formed quickly. This was allowed to stand for 1 hour, the white solid was separated by filtration, washed with water and air dried to give 5-methyl-2-nitro-N-(1H-tetrazol-5-yl)benzamide melting at about 278°-279° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04419357 |
| 出典データセット | uspto-grants-1983_12 |
| ORD ID | ord-a06f52ea2f434a8483b1c3bd8ca9c798 |
| 出典メモ | uspto-grants-1983_12 |