化工社化工社 化学情報印刷レポート · 研究参考用
Dimethylamine → 2-(2-Iodo-5-methoxyphenyl)-N,N-dimethylacetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | 2-(2-Iodo-5-methoxyphenyl)acetic acid | HCID 820071 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(2-Iodo-5-methoxyphenyl)-N,N-dimethylacetamide | HCID 14025497 | — |
反応手順
A 16.7 g (0.19 mole) sample of oxalyl chloride was added dropwise at 0° C. to a solution of 50.0 g (0.17 mole) of 2-iodo-5-methoxybenzeneacetic acid in 310 ml dry toluene and 31.7 ml of DMF. The mixture was allowed to warm to room temperature and stir for 16 hours. The solution was cooled to 0° C. and dimethylamine gas was admitted until the mixture was strongly basic. The mixture was allowed to warm to room temperature and stir for three hours and methylene chloride was added. The organic layer was washed with water, dilute hydrochloric acid, and sodium hydroxide. The organic layer was dried with MgSO4 and evaporated in vacuo to give 54.2 g of N,N-dimethyl-2-iodo-5-methoxybenzeneacetamide, mp 86°-89° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04725602 |
| 出典データセット | uspto-grants-1988_02 |
| ORD ID | ord-376b3b80298747838d4894a89b3c46a4 |
| 出典メモ | uspto-grants-1988_02 |