化工社化工社 化学情報印刷レポート · 研究参考用
Acetone → 6-Bromo-2,2-dimethyl-4H-benzo[d][1,3]dioxine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 5-Bromo-2-hydroxybenzyl alcohol | HCID 75342 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | 2,2-Dimethoxypropane | HCID 6495 | — |
| 生成物 | 6-Bromo-2,2-dimethyl-4H-benzo[d][1,3]dioxine | HCID 14520338 | — |
反応手順
To 5-bromo-2-hydroxybenzyl alcohol (93 g, 0.46 mol, available from Sigma-Aldrich) in 2.0 L of 2,2-dimethoxypropane was added 700 mL of acetone, followed by zinc chloride (170 g). After stirring for 18 hours, 1.0 M aqueous sodium hydroxide was added until the aqueous phase was basic. Diethyl ether (1.5 L) was added to the slurry and the organic phase was decanted into a separatory funnel. The organic phase was washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure to give the title compound as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07528253B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-24c3fb42e0934fb991e8732fbc4a985d |
| 出典メモ | uspto-grants-2009_05 |