참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | (2-Aminopropyl)hydrazine | HCID 13183609 | — |
| 반응물 | 2-Hydroxymethylene-5-methoxy-1-indanone | HCID 69754267 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | HCID 22338307 | HCID 22338307 | 20% |
반응 단계
To a solution of the product from Step A (1.9 g, 10 mmol) in ethanol (20 mL) was added a 1 N solution of HCl in a 1:1 mixture of methanol and ethanol followed by 2-aminopropylhydrazine (0.9 g, 10 mmol) and the solution was heated to reflux for 16 h. The solution was allowed to cool, poured into aqueous NaHCO3, extracted with ethyl acetate (2×20 mL), dried (Na2SO4) and concentrated. The crude material was taken up in 0.1 N HCl and washed with ether (2×20 mL), basified by the addition of NaHCO3 and extracted with ethyl acetate (2×20 mL). The combined organic extracts were dried (Na2SO4) and concentrated to a residue, which was purified by chromatography (silica, 10% methanol in dichloromethane) to furnish an oil (0.48 g, 20%); MS m/z 244 [M+H]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06933392B2 |
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| 출처 데이터셋 | uspto-grants-2005_08 |
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| ORD ID | ord-b32b2fde6e35495bbc4fc7a9f6a72dcc |
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| 출처 메모 | uspto-grants-2005_08 |
|---|