참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Tolylboronic acid | HCID 79799 | — |
| 반응물 | 5-(2-bromophenyl)-1-(4-nitrophenyl)-1H-tetrazole | HCID 19935790 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 5-(4'-Methyl[1,1'-biphenyl]-2-yl)-1-(4-nitrophenyl)-1H-tetrazole | HCID 19935776 | 95.1% |
반응 단계
A mixture of 4-methylphenyl boronic acid (9.7 g; 71 mmol), sodium carbonate (16.7 g; 158 mmol), water (100 ml), methanol (50 ml) and toluene (50 ml) was heated to 60° C. to give a clear solution. Compound C (20.0 g; 55 mmol) was then added, followed by tetrakis(triphenylphosphine)palladium (0.3 g; 0.25 mmol) and the mixture heated at reflux for 3 hours. Toluene (30 ml) was added and the warm mixture was filtered through diatomaceous earth. The organic phase was separated and the aqueous phase extracted with toluene (40 ml). The combined organic phases were evaporated to give a solid which was recrystallised from toluene/petroleum ether (100°-120° C.) (1:1 v/v) to give 5-(4'-methylbiphenyl-2-yl)-1-(4-nitrophenyl)-1H-tetrazole (D) (18.7 g; 90% yield), m.p. 164°-166° C.; NMR (CDCl3): 2.3(3H, s), 6.45(2H, d), 6.85(4H, m), 7.38(1H, d), 7.65(2H, m), 7.85(1H, d), 8.0(2H, d).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05420292 |
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| 출처 데이터셋 | uspto-grants-1995_05 |
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| ORD ID | ord-5550675d1eba484cac222c2c3626ffe1 |
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| 출처 메모 | uspto-grants-1995_05 |
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