関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Chlorobenzotrichloride | HCID 21277 | — |
| 反応物 | Chlorine | HCID 24526 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 3,4-Dichlorophenyltrichloromethane | HCID 25608 | 92% |
反応手順
In this apparatus, a mixture of 1,725 g (7.5 moles) of 4-chlorobenzotrichloride and 12 g (0.075 mole) of FeCl3 was heated to 70° C. and circulated. The introduction of 585 g (8.25 moles) of chlorine gas was then started. (chlorine gas was fed in at a rate such that no chlorine was detectable in the exit gas.) The reaction was complete after 5 hours. 2 liters of dilute hydrochloric acid were added to the reaction mixture and the organic phase was separated off, washed twice with 2 liters of water and dried over CaCl2. Subsequent fractional distillation gave 1,824 g of 3,4-dichlorobenzotrichloride (92% of theory) (98% purity according to a gas chromatogram), of boiling point 138°-140° C. at 12 mbar.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04769503 |
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| 出典データセット | uspto-grants-1988_09 |
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| ORD ID | ord-7b5fe7f8da4e4d218aa780c77a7ecd7d |
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| 出典メモ | uspto-grants-1988_09 |
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