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Ethyl levulinate → trans-6-Cyano-4-(I,6-dihydro-3-methyl-6-oxopyridazin-1-yl)-2,2-dimethylchroman-3-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl levulinate | HCID 10883 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | Benzyltrimethylammonium hydroxide | HCID 66854 | — |
| 反応物 | 6-methylpyridazin-3(2H)-one | HCID 83346 | — |
| 反応物 | 2,2-Dimethyl-3,4-epoxy-6-cyanochroman | HCID 10867360 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | trans-6-Cyano-4-(I,6-dihydro-3-methyl-6-oxopyridazin-1-yl)-2,2-dimethylchroman-3-ol | HCID 67823752 | 38.8% |
反応手順
A mixture is prepared which contains 1 g of 6-cyano-2,2-dimethyl-3,4-epoxychromane and 1.1 g of 6-methylpyridazin-3-one (prepared by the method described in J. Chem. Soc., 1947, p. 241, by reacting ethyl levulinate with hydrazine hydrate) in 10 ml of dioxane containing 0.1 ml of a 35% methanolic solution of benzyltrimethylammonium hydroxide. After 2 days at room temperature, the mixture is diluted with water and filtered, the material on the filter is dissolved in ethyl acetate, the water is then decanted and the organic phase is dried and concentrated. After recrystallization from an ethyl acetate/isopropyl ether mixture, 0.6 g of the expected product is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05284838 |
| 出典データセット | uspto-grants-1994_02 |
| ORD ID | ord-b77f316b6fdf4118aa48e5154e6ea792 |
| 出典メモ | uspto-grants-1994_02 |