化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Iodide → 2-Benzoyloxy-1,1-dimethoxy-ethane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2-Chloro-1,1-dimethoxyethane | HCID 60986 | — |
| 反応物 | Potassium Benzoate | HCID 23661960 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Benzoyloxy-1,1-dimethoxy-ethane | HCID 11608176 | 72.3% |
反応手順
Chloroacetaldehyde dimethyl acetal (50.0 g), potassium benzoate (70.7 g), potassium iodide (6.66 g) and DMF (N,N-dimethylformamide) (250 mL) were placed in a three-neck flask, followed by refluxing. Twenty hours later, the reaction mixture was cooled to room temperature, and water (250 mL) and ethyl acetate (250 mL) were added thereto, followed by stirring. After filtration, the filtrate was extracted with ethyl acetate (500 mL). The organic layer was subjected to vacuum concentration and then to vacuum distillation at 132-135° C. and at 5 mmHg and thereby yielded the target compound (61.0 g) in a yield of 72%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728152B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-fc9b9235d9cf49359251140b795631d9 |
| 出典メモ | uspto-grants-2010_06 |