関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl Methacrylate | HCID 6658 | — |
| 反応物 | Cyclohexanol | HCID 7966 | — |
| 反応物 | Potassium Cyanide | HCID 9032 | — |
| 反応物 | N,N'-Diphenylbenzidine | HCID 68280 | — |
| 反応物 | Methyl methacrylate methanol | HCID 19593510 | — |
| 生成物 | Cyclohexyl methacrylate | HCID 7561 | — |
反応手順
400 g of methyl methacrylate (4 mole), 200 g of cyclohexanol (2 mole) and 0.30 g of N,N'-diphenylbenzidine (500 ppm) are added to a 1 liter round-bottomed flask. Azeotropic dehydration is accomplished by conducting air through the resulting mixture, by way of a 1 m vigreux column. After cooling of the contents of the flask to about 75° C., 3 g of potassium cyanide (0.5%) are added, and the methyl methacrylate/methanol-azeotrope is distilled-off at a temperature of 65° C. at the head of the column. The trans-esterification is completed after 3.5 hours. After cooling of the flask, the sump is filtered to remove the potassium cyanide, and the filter residue is washed with a little methyl methacrylate. The filtrate is concentrated at 40° C. under a water jet vacuum. A residue of cyclohexyl methacrylate of 310 g = 85% will result.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04117238 |
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| 出典データセット | uspto-grants-1978_09 |
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| ORD ID | ord-19270db3b1b14bd99ccff77ff090aace |
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| 出典メモ | uspto-grants-1978_09 |
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