참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 2,6-Dichloro-4-nitroaniline | HCID 7430 | — |
| 반응물 | 4-Nitroaniline | HCID 7475 | — |
| 반응물 | Chlorine | HCID 24526 | — |
| 용매 | Nitric Acid | HCID 944 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Chloro-4-nitroaniline | HCID 8492 | 90% |
반응 단계
It has now been found that 2,6-dichloro-4-nitroaniline can be prepared in a high purity (purity of at least 96%) and a high yield (90% of theory) without the deficiencies mentioned, such as pollution of the effluent and technical effort for regeneration and working up of the effluent, by chlorination of 4-nitroaniline in water with chlorine bleaching liquor, by chlorinating 1 mole of 4-nitroaniline in 3-6 moles of hydrochloric acid (HCl) or nitric acid (HNO3) in the form of a dilute, aqueous acid in the presence of a dispersing agent which is stable under the reaction conditions, the chlorination initially being carried out at 5°-10° C. and then at 15-20° C. and, finally, after 90-95% of the 2-chloro-4-nitroaniline intermediately formed has been converted into 2,6-dichloro-4-nitroaniline, the temperature of the aqueous suspension being increased from 15°-20° C. to 70° C., without further addition of chlorine bleaching liquor and preferably with renewed addition of dispersing agent, and then by afterchlorinating, by renewed addition of chlorine bleaching liquor, at temperatures between 20° and 70° C., subsequently bringing the pH of the aqueous suspension to 9.0 and filtering off the 2,6-dichloro-4-nitroaniline formed and washing it with dilute mineral acid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04605767 |
|---|
| 출처 데이터셋 | uspto-grants-1986_08 |
|---|
| ORD ID | ord-c24e918046504812b1906301e4008f20 |
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| 출처 메모 | uspto-grants-1986_08 |
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