関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Cyanogen Bromide | HCID 10476 | — |
| 反応物 | 1,1-Bis(4-hydroxyphenyl)-2,2-dichloroethylene | HCID 84677 | — |
| 生成物 | 1,1-Dichloro-2,2-bis(4-cyanatophenyl)ethylene | HCID 11221227 | 98.2% |
反応手順
A 4-necked 5-L flask, equipped with a mechanical stirrer, a thermometer, and an additional funnel, is charged with methyl isobutyl ketone (1500 g), 1,1-dichloro-2,2-bis(4-hydroxyphenyl)ethene (320 g), and cyanogen bromide (270 g). The resulting solution is cooled to −20° C. with a dry ice/acetone bath. To the stirring solution, triethylamine (240 g) in the additional funnel is added dropwise. The reaction temperature is maintained below −20° C. After the addition, the resulting mixture is allowed to warm up to 0° C. and quenched with dilute HCl aqueous solution. The organic layer is washed further with water a few times and concentrated under vacuum to afford 370 g of amber liquid, which solidifies as light tan color solids.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06365671B1 |
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| 出典データセット | uspto-grants-2002_04 |
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| ORD ID | ord-d7d37a9766fe4341ae985fb8ab64f8a8 |
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| 出典メモ | uspto-grants-2002_04 |
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