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Triethylamine → 5,6-Dimethyl-4,5,6,7-tetrahydrothiazolo[4,5-d]pyridazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,2-Dimethylhydrazine dihydrochloride | HCID 9380 | — |
| 反応物 | 4,5-Bis(bromomethyl)thiazole | HCID 10849698 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5,6-Dimethyl-4,5,6,7-tetrahydrothiazolo[4,5-d]pyridazine | HCID 18442741 | — |
反応手順
Under ice cooling, 4,5-bis(bromomethyl)thiazole (600 mg) and 1,2-dimethylhydrazine dihydrochloride (294 mg) were suspended in ethanol (20 ml). Triethylamine (1.23 ml) was added in one portion to the reaction mixture, followed by stirring at room temperature for 30 minutes and then, at 50° C. for 30 minutes. The solvent was distilled off and the residue was purified by chromatography on a silica gel column (5% methanol—methylene chloride), whereby the title compound (90 mg, 24%) was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06747023B1 |
| 出典データセット | uspto-grants-2004_06 |
| ORD ID | ord-d27dc1db52c34ccfb27bdf9f7684590e |
| 出典メモ | uspto-grants-2004_06 |