化工社化工社 化学情報印刷レポート · 研究参考用
p-Toluenesulfonic acid monohydrate → 2-(5-Bromoindane-1-ylidene)-1,3-dithiane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 反応物 | 5-bromo-1-(1,3-dithian-2-yl)-2,3-dihydro-1H-inden-1-ol | HCID 57419484 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2-(5-Bromoindane-1-ylidene)-1,3-dithiane | HCID 57419485 | — |
反応手順
A mixture of (rac)-5-bromo-1-[1,3]dithian-2-yl-indan-1-ol (2.15 g, 6.49 mmol) and p-toluenesulfonic acid monohydrate (309 mg, 1.62 mmol) in benzene (30 ml) was heated to reflux for 2 h using a Dean-Stark trap to remove water. The brown solution was allowed to cool to room temperature and was diluted with sat. NaHCO3 solution. The layers were separated and the organic layer was washed with brine, dried with Na2SO4 and evaporated. The title compound was obtained as brown gum (2.024 g, 99%) and was used without purification for the next reaction step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08592426B2 |
| 出典データセット | uspto-grants-2013_11 |
| ORD ID | ord-074c5ef97fa1482094f2dbc5e672e221 |
| 出典メモ | uspto-grants-2013_11 |