참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium Azide | HCID 33557 | — |
| 반응물 | 1-Chloro-3-isocyanato-2-methylbenzene | HCID 2735770 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-(2-Methyl-3-chlorophenyl)-1,4-dihydrotetrazol-5-one | HCID 136646185 | 54.1% |
반응 단계
Under ice-cooling, to N,N-dimethylformamide 250 mL was added anhydrous aluminum chloride 21.9 g and the resulting mixtures were stirred for fifteen minutes. Thereto was added sodium azide 10.7 g and the resulting mixtures were stirred for fifteen minutes and thereto was then added 1-chloro-3-isocyanato-2-methylbenzene 25.0 g and the resulting mixtures were heated at 80° C. for five hours. After cooling the mixtures, to a mixture of sodium nitrite g, water 2 L and ice 500 g was added the reaction solutions with stirring. The mixtures were acidified with 10% hydrochloric acid and were extracted with ethyl acetate. The organic layers were washed with water and saturated saline, and were dried over anhydrous magnesium sulfate and were then concentrated under reduced pressure to give 1-(2-methyl-3-chlorophenyl)-1,4-dihydrotetrazole-5-one 17.0 g.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09380782B2 |
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| 출처 데이터셋 | uspto-grants-2016_07 |
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| ORD ID | ord-6dff5a3d4def4a8e94a9f4458b88d63d |
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| 출처 메모 | uspto-grants-2016_07 |
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