関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | Dimethyl 2-(2-methoxyphenoxy)malonate | HCID 12967085 | — |
| 反応物 | Pyridazine-3-carboximidamide hydrochloride | HCID 18756080 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178489618 | HCID 178489618 | — |
反応手順
Dimethyl 2-(2-methoxyphenoxy)malonate (3.05 g, 12.6 mmol) (Ref. Canadian Patent Application No. CA2071193A, 1992) in methanol (15 ml) was added over 5 minutes to a stirred, 25% w/v solution of sodium methoxide in methanol (8.58 ml, 37.8 mmol of sodium methoxide) at room temperature. The resulting mixture was stirred for 10 minutes and then a solution of 3-pyridazinecarboximidamide hydrochloride (2.0 g, 12.6 mmol) in methanol (15 ml) was added dropwise over 5 minutes and the resulting mixture was stirred at room temperature overnight. The reaction mixture was concentrated under vacuum and then diluted with water (100 ml). The aqueous solution was acidified to pH 4 with sulfuric acid (20%), resulting in the formation of the title compound as a purple solid, which was isolated by filtration (1.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06670362B2 |
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| 出典データセット | uspto-grants-2003_12 |
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| ORD ID | ord-5ae723d3be3a4c6f8eaf110aa2f6e70d |
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| 出典メモ | uspto-grants-2003_12 |
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