化工社化工社 化学情報印刷レポート · 研究参考用
p-Toluenesulfonic acid → 1-(2-Bromo-1,1-dimethoxyethyl)-2,4-dichlorobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Trimethyl orthoformate | HCID 9005 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Bromo-1-(2,4-dichlorophenyl)ethan-1-one | HCID 75828 | — |
| 反応物 | Calcium Chloride | HCID 5284359 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1-(2-Bromo-1,1-dimethoxyethyl)-2,4-dichlorobenzene | HCID 12705882 | 92% |
反応手順
A mixture of 13.5 parts of 2-bromo-1-(2,4-dichlorophenyl)ethanone, 5.5 parts of trimethoxymethane, 2 parts of 4-methylbenzenesulfonic acid and 80 parts of methanol is stirred and refluxed overnight (CaCl2 -tube). The reaction mixture is cooled and stirred for 30 minutes with 15 parts of a sodium hydroxide solution 50%. Then there are added 140 parts of 1,1'-oxybisethane and the mixture is washed with 300 parts of water. The organic phase is stirred with silica gel. The latter is filtered off and the filtrate is evaporated. The residue is dissolved in petroleumether. The solution is dried, filtered and evaporated, yielding 14.5 parts (92%) of 1-(2-bromo-1,1-dimethoxyethyl)-2,4-dichlorobenzene as a residue.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04160838 |
| 出典データセット | uspto-grants-1979_07 |
| ORD ID | ord-5d9d3edc7f09408389e305292b92e9b5 |
| 出典メモ | uspto-grants-1979_07 |