化工社化工社 化学情報印刷レポート · 研究参考用
Water → N,N'-dimethoxy-N,N'-dimethylbutanediamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Succinyl chloride | HCID 10970 | — |
| 反応物 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 生成物 | N,N'-dimethoxy-N,N'-dimethylbutanediamide | HCID 4379853 | — |
反応手順
Dissolve 136.2 g of succinyl dichloride and 180.0 g N,O-dimethylhydroxylamine hydrochloride in 1.2 L dichloromethane and cool it in an ice bath. Add 305.9 g pyridine from an addition funnel with stir over 1.5 hours. Let the reaction mixture warm up to room temperature over night. Pour the reaction mixture into ice and water and separate the layers. Wash the organic layer with cold 2 N HCl (2×), water, 5% NaHCO3 (2×), and saturated brine. Dry over anhydrous Na2SO4 and evaporate to give crude product. It was washed with 3:1 hexanes and dichloromethane and dried to give the title compound as a light tan solid 1H NMR (CDCl3, 500 MHz δ: 3.70 (s, 6H), 3.15 (s, 6H), 2.74 (s, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07528163B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-7fe6b6bc418f4397a56f52d339a64eeb |
| 出典メモ | uspto-grants-2009_05 |