참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Ethyl butyrimidate | HCID 16634 | — |
| 반응물 | 2-Ethoxybenzhydrazide | HCID 140788 | — |
| 반응물 | Ethyl butyrimidate hydrochloride | HCID 12235055 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 생성물 | HCID 178449906 | HCID 178449906 | — |
반응 단계
Ethyl butyrimidate hydrochloride from Example B (71.5 g, 472 mmol) is introduced into triethylamine (65 ml, 472 mmol) and cooled to 0° C. 2-Ethoxybenzohydrazide from Example A (85 g, 472 mmol) is suspended in 250 ml of isopropanol and added to the ethyl butyrimidate mixture. The reaction mixture is stirred at room temperature for 48 hours, the solid (triethylamine hydrochloride) is removed, and 25% strength hydrochloric acid (150 ml, 1.18 mol) is slowly added dropwise to the mother liquor at 0° C. to 5° C. The suspension of crystals is then stirred at 0° C. to 5° C. for 1 hour and the crystals are filtered with suction through a sintered funnel, washed with 100 ml of cold isopropanol and dried in a vacuum oven at 30° C. and 300 mbar overnight.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07022847B2 |
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| 출처 데이터셋 | uspto-grants-2006_04 |
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| ORD ID | ord-a662aa964a234715a1d7f3630eb82533 |
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| 출처 메모 | uspto-grants-2006_04 |
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