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Methanimidamide, hydrochloride (1:1) → HCID 178418881、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanimidamide, hydrochloride (1:1) | HCID 10313058 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | Dimethyl 2-(2-methoxyphenoxy)malonate | HCID 12967085 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178418881 | HCID 178418881 | 86.7% |
反応手順
At 5° C. sodium methylate (12.7 g) was added portionwise to a solution of dimethyl-(o-methoxyphenoxy)malonate (18.9 g) in methanol (450 ml). Upon completion of the addition stirring was continued at r.t. for 30 min followed by the addition of formamidine hydrochloride (6 g). The mixture was stirred at r.t. for 72 h. Eventually, the solvent was removed under reduced pressure and the remaining residue was suspended in diethyl ether. The solid material was filtered off and dissolved in water (100 ml). The solution was acidified with conc. hydrochloric acid. A white precipitate formed. The precipitate was collected, washed with water and dried to give 5-(o-methoxyphenoxy)-4,6-dihydroxy-pyrimidine (15.1 g) (or a tautomer) as a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094781B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-81e84f2f46764e7283256657b7d79e0f |
| 出典メモ | uspto-grants-2006_08 |