関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Dimethyl methoxymalonate | HCID 78718 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 4-(Benzyloxy)benzene-1-carboximidamide hydrochloride | HCID 11242483 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | HCID 178493927 | HCID 178493927 | 61.2% |
反応手順
A mixture of 85 g of 4-benzyloxybenzamidine hydrochloride, 78.6 g of dimethyl methoxymalonate, 1700 ml of ethanol, and 187 g of sodium methylate (28% methanol solution) was heated at 80° C. for 4 hours with stirring. After cooling, 1000 ml of acetic acid was slowly added to the reaction mixture, whereupon a yellow crystal precipitated. The precipitated crystals were collected by filtration, washed twice with water until the washing became neutral, and dried at 80° C. for 3 hours in high vacuo to obtain 64.2 g (percent yield: 60.7% ) of 4,6-dihydroxy-5-methoxy-2-(4-benzyloxyphenyl)pyrimidine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05290477 |
|---|
| 出典データセット | uspto-grants-1994_03 |
|---|
| ORD ID | ord-0676444237ca42619673ba1254c32ac4 |
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| 出典メモ | uspto-grants-1994_03 |
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