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Dabco → 1-(3,4-Dichlorobenzyl)-3-cyano-6-methylpyrid-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dabco | HCID 9237 | — |
| 反応物 | 3-Buten-2-one, 4-methoxy- | HCID 94297 | — |
| 反応物 | N-(3,4-dichlorobenzyl)-2-cyanoacetamide | HCID 4168883 | — |
| 溶媒 | 2-Methoxyethanol | HCID 8019 | — |
| 生成物 | 1-(3,4-Dichlorobenzyl)-3-cyano-6-methylpyrid-2-one | HCID 20316351 | 62% |
反応手順
A solution of 49.7 g. (0.204 mole) of N-(3,4-dichlorobenzyl)-2-cyanoacetamide, 48.0 g. (0.48 mole) of 4-methoxy-3-buten-2-one, and 4 g. of 1,4-diazabicyclo (2.2.2) octane (DABCO) in 160 ml. of 2-methoxyethanol is refluxed for 4 hr. The dark reaction mixture is then concentrated in vacuo and the crude solid is isolated by filtration from the resulting slurry and washed with ether. The crude product is dissolved in methylene chloride and the organic solution is washed with water, 2N-HCl and finally with more water. The methylene chloride is removed and the product is obtained in 62% yield by ether trituration.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04028084 |
| 出典データセット | uspto-grants-1977_06 |
| ORD ID | ord-8676f4fd4901411d9d023b915b59605f |
| 出典メモ | uspto-grants-1977_06 |