참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | O-Phenylenediamine | HCID 7243 | — |
| 반응물 | 2-Propenoic acid, 3,3-diethoxy-, ethyl ester | HCID 169388 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 2H-1,5-Benzodiazepin-2-one, 4-ethoxy-1,3-dihydro- | HCID 58957915 | 56.5% |
반응 단계
To a solution phenylenediamine (17.2 g, 159.2 mmol) and acetic acid (0.4 mL) in xylenes (225 mL) at 140° C. was added 3,3-diethoxyacrylic acid ethyl ester (30.0 g, 159.2 mmol) in xylenes (80 mL) dropwise over 50 minutes. The reaction was heated at 140° C. for 2 hours, was cooled to room temperature, and was stirred for 24 h. The resulting white precipitate was filtered, was washed with ether (100 mL), and was dried under vacuum to provide 18.37 g of 4-ethoxy-1,3-dihydro-benzo[b][1,4]diazepin-2-one as a white fluffy solid. MS 205 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07265104B2 |
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| 출처 데이터셋 | uspto-grants-2007_09 |
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| ORD ID | ord-212100e82c624273907b2684f40afc23 |
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| 출처 메모 | uspto-grants-2007_09 |
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