関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propylene Oxide | HCID 6378 | — |
| 反応物 | 5-Tert-butyl-m-xylene | HCID 7378 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Bromo-5-tert-butyl-1,3-dimethylbenzene | HCID 220364 | 89.3% |
反応手順
To a solution of 200 g (1.23 mole) 5-t-butyl-1,3-dimethylbenzene and 83 ml (1.23 mole) propylene oxide in 500 ml of methylene chloride at 15° C. or less, 63 ml (1.23 mole) bromine was added dropwise while maintaining the solution temperature at 15° C. or less. The reaction mixture was allowed to warm to 25° C. overnight. A 200 ml solution of 5% by weight of potassium hydroxide in water was added and the resulting two phase system was stirred for 1 hr at 25° C. The organic phase was washed with water and dried over anhydrous magnesium sulfate. After solvent evaporation an oil was left which when crystallized from methanol gave 265 g (87% yield) of the title compound after drying in vacuo. The oil could also be purified by distilling at 61°-70° C. under a reduced pressure of 0.25 mm of mercury.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04777270 |
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| 出典データセット | uspto-grants-1988_10 |
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| ORD ID | ord-738fe73501f0484cb7b8643d628aeb3a |
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| 出典メモ | uspto-grants-1988_10 |
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