関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2-Chloro-5-nitrobenzoic acid | HCID 17287 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Chloro-5-nitrobenzamide | HCID 286562 | — |
反応手順
A mixture of 2-chloro-5-nitrobenzoic acid (15.0 g, 74.0 mmol) in 200 mL of dichloromethane was reacted at 24° C. with oxalyl chloride (16.2 mL, 186.0 mmol) and a catalytic amount of dimethylformamide. After 3 hours, the solvent was removed in vacuo, and the residue was redissolved in 200 mL of fresh dichloromethane. The solution was cooled to 0° C., and ammonia was bubbled into the solution for 5 minutes, whereupon the product precipitated from solution. The product was collected by filtration to yield 6.8 g of 2-chloro-5-nitro benzamide, mp 174°-175° C.;
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05734081 |
|---|
| 出典データセット | uspto-grants-1998_03 |
|---|
| ORD ID | ord-2c2bf9e31bb848cdbaf04402697bce42 |
|---|
| 出典メモ | uspto-grants-1998_03 |
|---|