関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | ethyl 4,6-dimethyl-2-oxo-2H-pyran-5-carboxylate | HCID 76918 | — |
| 反応物 | Hydrazinium chloride | HCID 115031 | — |
| 溶媒 | Potassium Carbonate | HCID 11430 | — |
| 生成物 | HCID 58307466 | HCID 58307466 | 7% |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08207347B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-cafca3c763bb4a119ded67a4451b45ac |
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| 出典メモ | uspto-grants-2012_06 |
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