関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | 2-Propenoic acid, 3,3-diethoxy-, ethyl ester | HCID 169388 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | Benzamidine HCl hydrate | HCID 16219042 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 6-Ethoxy-2-phenylpyrimidin-4(3H)-one | HCID 608431 | 57% |
反応手順
A mixture of 3.14 g (20.0 mmol) of benzamidine hydrochloride hydrate, 1.65 g (20.1 mmol) of powdered anhydrous sodium acetate, 4.17 g (22.2 mmol) of ethyl 3,3-diethoxyacrylate and 10 mL of DMSO was heated at 120° C. for 8 h. The mixture was cooled, diluted with 50 mL of 5% aqueous NaOH and washed with two 100 mL portions of ether. The aqueous layer was acidified with concentrated hydrochloric acid and the precipitate was collected by filtration and dried under vacuum at 50° C. to furnish 2.28 g (57%) of crude 6-ethoxy-2-phenyl-4(3H)-pyrimidinone as a yellow solid 1 H-NMR (d6-DMSO) δ 1.35(3H,t), 4.33(2H,q), 5.60(1H,s), 7.50(3H,m), 8.2(2H,m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05726124 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-2b0378d7412b4bedb3ed0ed2242b2a38 |
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| 出典メモ | uspto-grants-1998_03 |
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