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 hydrochloride | HCID 134414 | — |
| 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 | 24% |
反応手順
After 4,5-bis(bromomethyl)thiazole (600 mg) synthesized in 1) of Referential Example 109 was dissolved in ethanol (20 ml), and 1,2-dimethylhydrazine hydrochloride (294 mg) was added under ice cooling, triethylamine (1.23 ml) was added at a time, and the mixture was stirred for 30 minutes at room temperature and 30 minutes at 50° C. The solvent was distilled off, and the residue was purified by column chromatography on silica gel (methanol:dichloromethane=1:19) to obtain 5,6-dimethyl-4,5,6,7-tetrahydrothiazolo[4,5-d]-pyridazine (90 mg) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07192968B2 |
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| 出典データセット | uspto-grants-2007_03 |
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| ORD ID | ord-991b27bbedf14179a68243c37f5545e2 |
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| 出典メモ | uspto-grants-2007_03 |
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