関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoyl chloride | HCID 7412 | — |
| 反応物 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 反応物 | m-Bromobenzohydrazide | HCID 520941 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Benzoic acid, m-bromo-, benzoylhydrazide | HCID 52256 | 96% |
反応手順
Subsequently, 5.0 g (23 mmol) of 3-bromobenzohydrazine obtained in (i) above was put in a 300-mL three-neck flask, 10 mL of N-methyl-2-pyrrolidone was added therein, and the mixture was stirred. Thereafter, a mixed solution of 10 mL of N-methyl-2-pyrrolidone and 3.2 mL (28 mmol) of benzoyl chloride was dripped to the above mixture through a 50-mL dropping funnel. After the dripping, the mixture was heated and stirred at 80° C. for 3 hours so as to be reacted. After the reaction, water was added to the reaction solution, and a solid was precipitated. The precipitated solid was collected by suction filtration to obtain another solid. The obtained solid was washed with approximately 1 L of water and collected by suction filtration. The collected solid was washed with methanol and collected by suction filtration; thus, 7.1 g of a white solid that was an object was obtained (yield: 96%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09048436B2 |
|---|
| 出典データセット | uspto-grants-2015_06 |
|---|
| ORD ID | ord-88045fea0820467db4c0fd90dcf48384 |
|---|
| 出典メモ | uspto-grants-2015_06 |
|---|