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Hydrazine hydrate (1:1) → N-{1-[3-(4-Methylbenzyl)-5-oxo-4,5-dihydro-1,2,4-triazin-6-yl]ethyl}acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | Benzeneethanimidamide, 4-methyl-, hydrochloride (1:1) | HCID 13430819 | — |
| 反応物 | Ethyl 3-acetamido-2-oxobutanoate | HCID 22245807 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | N-{1-[3-(4-Methylbenzyl)-5-oxo-4,5-dihydro-1,2,4-triazin-6-yl]ethyl}acetamide | HCID 135697912 | — |
反応手順
10 g (54.2 mmol) of 2-(4-methylphenyl)ethanamidine hydrochloride (Example 3A) are taken up in 100 ml of ethanol and treated with 3.25 g (65.0 mmol) of hydrazine hydrate. The mixture is stirred for 45 min, then the compound of Example 6A is added. It is then stirred for 4 h at 80° C. (bath) and overnight at room temperature. The substance is purified by flash chromatography, preliminary fractions first being separated off using ethyl acetate. The product is eluted with dichloromethane/methanol 30/1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06998402B2 |
| 出典データセット | uspto-grants-2006_02 |
| ORD ID | ord-c9a112bf58034991869e037381cd0f8a |
| 出典メモ | uspto-grants-2006_02 |