참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 3-Bromo-4-isopropylaniline | HCID 280799 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 촉매 | Sulfamic Acid | HCID 5987 | — |
| 촉매 | Cuprous chloride | HCID 62652 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Bromo-4-chloro-1-(1-methylethyl)benzene | HCID 67988282 | 62.3% |
반응 단계
Hydrochloric acid (152 g, 31% strength, 1.29 mol) was added dropwise to a suspension of 3-bromo-4-isopropylaniline (VII) (100 g, 0.43 mol) and water (150 g) at room temperature. The suspension was subsequently cooled to 5° C. and a solution of sodium nitrite (32.7 g, 0.46 mol) in water (140 g) was added dropwise over a period of 2 hours. After stirring for another 1 hour, amidosulphuric acid (2.5 g, 0.026 mol) was added. Copper(I) chloride (10.8 g, 0.11 mol), hydrochloric acid (202 g, 31%, 1.72 mol) and water (75 g) were placed in a second flask and the diazonium salt generated previously was added dropwise over a period of 30 minutes. After stirring for another 1.5 hours, the mixture was extracted with dichloromethane (250 g), the phases were separated and dichloromethane was distilled off under reduced pressure. The crude product obtained was purified by distillation. 2-Bromo-4-chloro-1-isopropylbenzene (62.6 g, 94.8 GC-% by area. 59% of theory) was obtained as a colourless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09440908B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-75e5646be5c9480fba177cf39bd72a36 |
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| 출처 메모 | uspto-grants-2016_09 |
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