化工社化工社 化学情報印刷レポート · 研究参考用
Nitric Acid → 3-Acetamido-4-methyl-2-nitrobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | 3-Acetamido-4-methylbenzoic acid | HCID 243432 | — |
| 生成物 | 3-Acetamido-4-methyl-2-nitrobenzoic acid | HCID 243433 | 63% |
反応手順
3-Acetamido-4-methylbenzoic acid (205 g, 1061 mmol) was added portionwise over 45 min to stirred fuming nitric acid (1 L) at −5° C., maintaining a reaction temperature below 0° C. The mixture was stirred for an additional 1 h and then crushed ice (2.5 kg) was added. The mixture was stirred for a further 30 min. The precipite that formed was filtered off and thoroughly washed with water. The resulting cake was air dried and suspended in 1 L of acetic acid at 65° C. The suspension was stirred for 1 hour, allowed to cool down to RT and then filtered. The filtrate was washed with acetic acid and ether to give 3-acetamido-4-methyl-2-nitrobenzoic acid (160 g, 63%) as a white solid. MS (M+H)+ 239.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07989461B2 |
| 出典データセット | uspto-grants-2011_08 |
| ORD ID | ord-211ad1ef95614473accc3acc8d2750c0 |
| 出典メモ | uspto-grants-2011_08 |