참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1-(2-Methyl-3-chlorophenyl)-1,4-dihydrotetrazol-5-one | HCID 136646185 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-(2-Methyl-3-chlorophenyl)-4-methyl-1,4-dihydrotetrazol-5-one | HCID 89875342 | — |
반응 단계
To a mixture of the above-mentioned 1-(2-methyl-3-chlorophenyl)-1,4-dihydrotetrazole-5-one 10.00 g and N,N-dimethylformamide 100 mL was added 55% sodium hydride 2.30 g under ice-cooling. The mixtures were raised to room temperature and were stirred for one hour. To the reaction mixtures was added methyl iodide 3.2 mL under ice-cooling. The mixtures were raised to room temperature and were stirred for fourteen hours. To the reaction mixtures was added water and the mixtures were extracted with ethyl acetate. The organic layers were washed with 10% hydrochloric acid, water and saturated saline, and were dried over anhydrous magnesium sulfate and were then concentrated under reduced pressure. The resulting residues were subjected to a silica gel column chromatography to give 1-(2-methyl-3-chlorophenyl)-4-methyl-1,4-dihydrotetrazole-5-one (hereinafter, referred to as “Intermediate (PRC-P)”) 1.56 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-403e7a438de74a10aec040243e727c0b |
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| 출처 메모 | uspto-grants-2016_07 |
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