関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Bromo-2,5-furandione | HCID 80027 | — |
| 反応物 | 4-Methoxybenzylhydrazine hydrochloride | HCID 45789374 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 90419128 | HCID 90419128 | — |
反応手順
(4-methoxybenzyl)hydrazine hydrochloride (2.132 g, 11.30 mmol) and 3-bromofuran-2,5-dione (2 g, 11.30 mmol) in water (20 ml) was stirred and heated at 100° C. overnight. The mixture was cooled to room temperature and filtered to collect the solid. The solid was triturated with a mixture of ethyl acetate and ethyl ether (1/4) and the mixture was filtered. The insoluble residue was 4-bromo-1-(4-methoxybenzyl)-1,2-dihydropyridazine-3,6-dione. LRMS m/z (M+H) 311.0 found, 311.0 required. The filtrate was concentrated in vacuo and the residue was purified by column chromatography on silica gel (Petroleum ether: ethyl acetate=1/1)) to give 5-bromo-1-(4-methoxybenzyl)-1,2-dihydropyridazine-3,6-dione. LRMS m/z (M+H) 311.0 found, 311.0 required.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09353104B2 |
|---|
| 出典データセット | uspto-grants-2016_05 |
|---|
| ORD ID | ord-1d7cd40a9392450cbe486614f9434826 |
|---|
| 出典メモ | uspto-grants-2016_05 |
|---|