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Diethyl Malonate → HCID 178489012、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Malonate | HCID 7761 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 4-Methoxybenzamidine Hydrochloride | HCID 12326219 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178489012 | HCID 178489012 | 83.9% |
反応手順
338 g of a 30% solution of sodium methylate in methanol are added over 10 minutes to a suspension of 112 g of p-methoxybenzamidine hydrochloride and 101 g of diethyl malonate in 520 ml of ethanol, and the mixture is subsequently refluxed for 5 hours. The reaction mixture is then concentrated by rotary evaporation and the residue is dissolved in 1000 ml of warm water of 80° C. The solution is filtered and the filtrate is acidified to pH 1. The precipitate is isolated by filtration and vacuum dried at 80° C., affording 109.8 g of 2-p-methoxyphenyl-4,6-dihydroxypyrimidine with a melting point of 318° C. (decompos.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04674229 |
| 出典データセット | uspto-grants-1987_06 |
| ORD ID | ord-9bd82115635c44efbcd6ea8d55ec29a4 |
| 出典メモ | uspto-grants-1987_06 |