化工社化工社 化学情報印刷レポート · 研究参考用
N-methylhydroxylamine hydrochloride → 7-Acetyl-1,2-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-methylhydroxylamine hydrochloride | HCID 77906 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | N-allyl-N-(2-oxopropyl)-acetamide | HCID 15069994 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 7-Acetyl-1,2-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane | HCID 15070017 | — |
反応手順
15.5 g (0.1 mol) of N-allyl-N-(2-oxopropyl)-acetamide are dissolved in 100 ml of dioxane, and 9 g of anhydrous sodium acetate and 9 g (0. 108 mol) of N-methylhydroxylamine hydrochloride in 10 ml of water are added. The mixture is heated under reflux overnight and cooled and the salts are filtered off with suction and washed with dioxane. The filtrate is concentrated, the residue is taken up in 100 ml of water and K2CO3 is added. The mixture is extracted with CHCl3, the extract is dried over K2CO3 and concentrated and the residue is distilled.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05416096 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-e9c25c5ffd3943a2b66fece54b978100 |
| 出典メモ | uspto-grants-1995_05 |