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Acetone → 5,5-Bis(bromomethyl)-2,2-dimethyl-1,3-dioxane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 2,2-Bis(bromomethyl)-1,3-propanediol | HCID 18692 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 5,5-Bis(bromomethyl)-2,2-dimethyl-1,3-dioxane | HCID 14537228 | — |
反応手順
A mixture of 10 g of 2,2-bis(bromomethyl)-1,3-propanediol, 5 ml of acetone and a catalytic quantity (0.1 g) of p-toluenesulfonic acid was heated under reflux in 150 ml of benzene until the theoretical amount of water (0.8 ml) had been collected in a Dean-Stark trap (2 hours). Evaporation of the solvent gave 5,5-bis(bromomethyl)-2,2-dimethyl-1,3-dioxane (6A), as a solid, m.p.: 56°-58° C. The purity according to gas-liquid chromatography and proton NMR was 99%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04665197 |
| 出典データセット | uspto-grants-1987_05 |
| ORD ID | ord-994df256764a44c08adbb3675f3fd28f |
| 出典メモ | uspto-grants-1987_05 |