関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Chlorobenzoic Acid | HCID 447 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 2-Oxocyclohexanepropiononitrile | HCID 96223 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 3-Chlorobenzoic Acid | HCID 447 | — |
| 生成物 | 3-(7-Oxooxepan-2-yl)propanenitrile | HCID 11768938 | — |
反応手順
A reactor is loaded with 151 g of 3-(2-cyclohexanonyl)propionitrile in 500 ml of n-hexane and 260 g of m-chloroperbenzoic acid (70% titer) dissolved at 50° C. in 2000 ml of n-hexane in 30 minutes. The solution is heated to 55° C. for 15 hours. Cooling of the solution separates, in crystalline form, part of the m-chlorobenzoic acid which is scarcely soluble in the system, together with a heavy liquid phase which is formed by 7-cyanoethyl-2-oxepanone and by m-chlorobenzoic acid. 71.5 g of 7-cyanoethyl-2-oxepanone, impure with m-chlorobenzoic acid, are recovered from the lower phase. 24 g of 7-cyanoethyl-2-oxepanone are recovered from the upper phase by concentration and several crystallizations. Conversion over the initial ketone is 85%. Yield on the converted amount is 57%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05872267 |
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| 出典データセット | uspto-grants-1999_02 |
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| ORD ID | ord-08b32fbbc1ad4e3a8e50204892016904 |
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| 出典メモ | uspto-grants-1999_02 |
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