関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Oxygen | HCID 977 | — |
| 反応物 | 2-Chlorotoluene | HCID 7238 | — |
| 反応物 | Epichlorohydrin | HCID 7835 | — |
| 触媒 | Cobalt octoate | HCID 8696 | — |
| 生成物 | 2-Chlorobenzoic Acid | HCID 8374 | — |
反応手順
Into the column described in Example 1 were charged 453 grams (3.58 moles) of o-chlorotoluene, 2.25 grams of cobalt octoate (6% Co), and 2.25 grams of epichlorohydrin. The reaction mixture was heated to 155° C. and maintained at that temperature while oxygen that had been sparged through epichlorohydrin was bubbled through it at the rate of 200 ml./min. Throughout the reaction period, the gases leaving the reactor remained non-acidic. At the end of 23 hours, the reaction mixture was removed from the column, cooled to 75° C., and extracted with 600 grams of 10 percent aqueous sodium hydroxide solution. The layers that formed were separated. The aqueous layer was diluted with water to a volume of 1500 ml. and then acidified with hydrochloric acid. The o-chlorobenzoic acid that precipitated was collected, washed with water, and dried. There was obtained 180 grams (1.155 moles) of o-chlorobenzoic acid. The conversion of o-chlorotoluene to o-chlorobenzoic acid was 14 percent. The yield of o-chlorobenzoic acid, based on o-chlorotoluene reacted, was 78.6 percent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04034007 |
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| 出典データセット | uspto-grants-1977_07 |
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| ORD ID | ord-ac39148028b44a73bcdd872445048803 |
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| 出典メモ | uspto-grants-1977_07 |
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