関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Octylamine | HCID 8143 | — |
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | rac-(1R,2R)-2-(4-nitrophenyl)cyclopropane-1-carboxylic acid | HCID 12854631 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | trans-N-Octyl-2-(4-nitrophenyl)cyclopropanecarboxamide | HCID 12854633 | — |
反応手順
To a stirred slurry of 4.1 g. of trans-2-(4-nitrophenyl)cyclopropanecarboxylic acid in 50 ml. of chloroform was added 2.2 g. of triethylamine. The clear solution thus obtained was cooled to ca. 5° C., and a solution of 2.4 g. of ethyl chloroformate in 15 ml. of chloroform was added dropwise with stirring during 15 minutes. Stirring was continued for 20 minutes, and then a solution of 2.8 g. of octylamine in 15 ml. of chloroform was added dropwise with stirring, at 0°-5° C., during 10-15 minutes. The cooling bath was removed, and stirring was continued for 1 hour. At this point, the solvent was removed by evaporation in vacuo, and the residue was triturated under a mixture of 70 ml. of water and 15 ml. of ethanol. The solid which remained out of solution was recovered by filtration, washed with water, and dried, to give 6.2 g. of the title compound as a white solid, m.p. 126° -129° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04343813 |
|---|
| 出典データセット | uspto-grants-1982_08 |
|---|
| ORD ID | ord-392ee65cf4244ebc867e6abbcd49cb68 |
|---|
| 出典メモ | uspto-grants-1982_08 |
|---|