関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,6-Dichloro-4-methylpyridazine | HCID 87923 | — |
| 反応物 | 2,4-Dimethoxybenzylamine | HCID 597250 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | (6-Chloro-5-methyl-pyridazin-3-yl)-(2,4-dimethoxy-benzyl)-amine | HCID 86696398 | 28% |
反応手順
A mixture of 3,6-dichloro-4-methylpyridazine (1.35 g, 8.28 mmol) and 2,4-dimethoxybenzylamine (11.1 g, 66.3 mmol) in i-PrOH (5 ml) was heated in a microwave at 100° C. for 50 min. (30+20 min.). The mixture was concentrated and the residue was subjected to ISCO (120 g column, hexane 5 min., 0-55% EtOAc in hexane over 90 min. to give (6-chloro-5-methyl-pyridazin-3-yl)-(2,4-dimethoxy-benzyl)-amine (680 mg) plus the 6-methyl analog (320 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08969565B2 |
|---|
| 出典データセット | uspto-grants-2015_03 |
|---|
| ORD ID | ord-3b5c47ff103249a2ba6ebcf424168253 |
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| 出典メモ | uspto-grants-2015_03 |
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