참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | tert-Butanol | HCID 6386 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 반응물 | 2-(Benzyloxy)-4-chlorobenzoic acid | HCID 22452154 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-benzyloxy-4-chloro-N-tert-butoxycarbonylaniline | HCID 22010963 | — |
반응 단계
To a solution of 2-benzyloxy-4-chlorobenzoic acid (12.9 g, 46.6 mmol), t-butanol (17.5 mL, 186 mmol) and triethylamine (7.79 mL, 55.9 mmol) in toluene (250 mL) is added DPPA (11.1 mL, 51.3 mmol) and the mixture is stirred at 85° C. for 3 h then at 65° C. for 48 h. The mixture is diluted with EtOAc (500 mL) and is washed with 1N HCl (3×150 mL), NaHCO3 (3×150 mL) and brine (150 mL). The organic phase is dried over sodium sulfate and the solvent evaporated to give a brown solid which is triturated with hexane to give the title compound: (M−1)−=332.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08084448B2 |
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| 출처 데이터셋 | uspto-grants-2011_12 |
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| ORD ID | ord-d9458652188140359ec8df881f4c9e69 |
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| 출처 메모 | uspto-grants-2011_12 |
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