化工社化工社 化学情報印刷レポート · 研究参考用
Water → 2-Carbobutoxyethyl-2-methyl-5-nitro-5-ethyl-1,3-dioxane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Ethyl-2-nitro-1,3-propanediol | HCID 11696 | — |
| 反応物 | Butyl levulinate | HCID 16331 | — |
| 触媒 | p-Toluenesulfonic acid | HCID 6101 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Carbobutoxyethyl-2-methyl-5-nitro-5-ethyl-1,3-dioxane | HCID 18996043 | 90% |
反応手順
7.46 g of 2-nitro-2-ethyl-1,3-propanediol, 8.61 g of butyl levulinate, 50 mg of p-toluenesulfonic acid in 50 ml of toluene was refluxed until no more water separated. The reaction mixture was cooled, washed with 2% sodium bicarbonate and water, dried and concentrated to give 13.65 g of 2-carbobutoxyethyl-2-methyl-5-nitro-5-ethyl-1,3-dioxane as a light yellow oil. This was dissolved in 50 ml of ethanol and hydrogenated over 1 g Raney Nickel catalyst at 60 under pressure. Distillation of the crude material at 160° C./3mm gave 11 g of the product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05482965 |
| 出典データセット | uspto-grants-1996_01 |
| ORD ID | ord-b6d8796fb6b5473fabc0bfadfb20ba01 |
| 出典メモ | uspto-grants-1996_01 |