참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | tert-Butanol | HCID 6386 | — |
| 반응물 | p-Nitroacetophenone | HCID 7487 | — |
| 반응물 | Diethylamine | HCID 8021 | — |
| 반응물 | 2-Bromo-4'-nitroacetophenone | HCID 66840 | — |
| 촉매 | Zincchloride | HCID 3007855 | — |
| 용매 | Benzene | HCID 241 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1,4-Bis(4-nitrophenyl)butane-1,4-dione | HCID 13762891 | 61% |
반응 단계
Anhydrous zinc(II)chloride (2.73 g, 20.00 mmol) was stirred in dry benzene (15 mL) while diethylamine (1.558 mL, 15.00 mmol) and t-butanol (1.435 mL, 15.00 mmol) were added, and the resulting mixture was stirred at room temperature for 90 minutes to give a cloudy solution. To this mixture was added 2-bromo-1-(4-nitrophenyl)ethanone (2.44 g, 10.00 mmol) and 1-(4-nitrophenyl)ethanone (2.477 g, 15.00 mmol), and the resulting mixture was stirred at room temperature overnight. The mixture was poured into water (50 mL) and extracted with ethyl acetate (3×50 mL). The combined organic layers were dried over Na2SO4, filtered and concentrated. The resulting residue was triturated with dichloromethane to give an orange solid that was collected by filtration and dried to give the title compound (2.0 g, 61% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08937150B2 |
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| 출처 데이터셋 | uspto-grants-2015_01 |
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| ORD ID | ord-bb7dd1484fe249dba2bb0aee9556ffbf |
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| 출처 메모 | uspto-grants-2015_01 |
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