化工社化工社 化学情報印刷レポート · 研究参考用
Isopropylamine → 3-methyl-N-(1-methylethyl)-2-nitrobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isopropylamine | HCID 6363 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | 3-Methyl-2-nitrobenzoic acid | HCID 21575 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-methyl-N-(1-methylethyl)-2-nitrobenzamide | HCID 890272 | 80.2% |
反応手順
A solution of 3-methyl-2-nitrobenzoic acid (2.00 g, 11.0 mmol) and triethylamine (1.22 g, 12.1 mmol) in 25 mL of methylene chloride was cooled to 10° C. Ethyl chloroformate was carefully added and a solid precipitate formed. After stirring for 30 minutes isopropylamine (0.94 g, 16.0 mmol) was added and a homogeneous solution resulted. The reaction was stirred for an additional hour, poured into water and extracted with ethyl acetate. The organic extracts were washed with water, dried over magnesium sulfate and evaporated under reduced pressure to afford 1.96 g of the desired intermediate as a white solid melting at 126-128° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06747047B2 |
| 出典データセット | uspto-grants-2004_06 |
| ORD ID | ord-8004850695024a47a29bb1b3da16a6c8 |
| 出典メモ | uspto-grants-2004_06 |