참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzenecarboximidic acid, ethyl ester, hydrochloride (1:1) | HCID 79249 | — |
| 반응물 | 5-Methyl-3-phenyl-4-isoxazolecarbohydrazide | HCID 727924 | — |
| 반응물 | Sodium ethoxide | HCID 2723922 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | HCID 16722532 | HCID 16722532 | 58.4% |
반응 단계
To a solution of ethyl benzimidate hydrochloride (376 mg; 2.03 mmol) in ethanol (4 mL) was added at 0° C. sodium ethoxide (2.72 M in ethanol, 355 □L, 0.99 mmol) and stirred for 15 min. The suspension was filtered off and 5-methyl-3-phenyl-isoxazole-4-carboxylic acid hydrazide (200 mg, 0.92 mmol) was added and stirred for 90 h at 70° C. The reaction mixture was suspended in dioxane (4 mL) and heated in the microwave for 30 min at 180° C. Concentration and then purification by chromatography (SiO2, heptane:ethyl acetate=95:5 to 60:40) afforded the title compound (163 mg, 29%) as a white solid. MS: m/e=304.2 [M+H]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07541372B2 |
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| 출처 데이터셋 | uspto-grants-2009_06 |
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| ORD ID | ord-593f269607994f9ca762e99580f58b38 |
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| 출처 메모 | uspto-grants-2009_06 |
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