関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5-Methylisatoic anhydride | HCID 294478 | — |
| 反応物 | Alanine, methyl ester, hydrochloride (1:1) | HCID 2756298 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 3,4-dihydro-3,7-dimethyl-1H-1,4-benzodiazepine-2,5-dione | HCID 21251942 | 50.5% |
反応手順
A mixture of 17.7 parts of 6-methyl-4H-3,1-benzoxazine-2,4(1H)-dione, 15.0 parts of methyl 2-aminopropanoate monohydrochloride and 62.7 parts of pyridine was refluxed for 6 hours under argon. The reaction mixture was cooled at -10° C. for 1 hour. The precipitate was filtered off, rinsed with water, triturated in ethanol and rinsed with ethanol and 1,1'-oxybisethane, yielding 10.32 parts (50.5%) of 3,4-dihydro-3,7-dimethyl-1H-1,4-benzodiazepine-2,5-dione (interm. 43).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05270464 |
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| 出典データセット | uspto-grants-1993_12 |
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| ORD ID | ord-f7165850443545da827498134458d007 |
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| 出典メモ | uspto-grants-1993_12 |
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