참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | ethyl 4,6-dimethyl-2-oxo-2H-pyran-5-carboxylate | HCID 76918 | — |
| 반응물 | Hydrazinium chloride | HCID 115031 | — |
| 용매 | Potassium Carbonate | HCID 11430 | — |
| 생성물 | HCID 58307466 | HCID 58307466 | 7% |
반응 단계
A mixture of 4,6-dimethyl-2-oxo-2H-pyran-5-carboxylic acid ethyl ester (3.2 mL, 19 mmol) and hydrazine monohydrochloride (1.4 g, 20 mmol) in methanol (16 mL, 0.39 mmol) was heated under microwave irradiation for 2.5 hrs at 150° C. Reaction was taken up in sat. aq. K2CO3 (40 mL) and extracted with ethyl acetate (3×40 mL). The combined organic phases were washed with brine, dried over MgSO4, evaporated and purified by flash chromatography. Yield 7%. 1H NMR (500 MHz, CDCl3): 6.35 (s, 1H), 5.12 (s, 2H), 4.35 (q, J=7.1 Hz, 2H), 2.53 (s, 3H), 2.21 (s, 3H), 1.37 (t, J=7.1 Hz, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08207347B2 |
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| 출처 데이터셋 | uspto-grants-2012_06 |
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| ORD ID | ord-cafca3c763bb4a119ded67a4451b45ac |
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| 출처 메모 | uspto-grants-2012_06 |
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