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HRID 451371作成日:2026年10月25日
1,4-Dioxa-8-azaspiro(4.5)decane → 8-(3-Methyl-[1,2,4]thiadiazol-5-yl)-1,4-dioxa-8-aza-spiro[4.5]decane
https://huagongshe.com/reaction/451371
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,4-Dioxa-8-azaspiro(4.5)decane | HCID 67435 | — |
| 反応物 | 2-(Dicyclohexylphosphino)biphenyl | HCID 2734216 | — |
| 反応物 | 5-Chloro-3-methyl-1,2,4-thiadiazole | HCID 12919159 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 8-(3-Methyl-[1,2,4]thiadiazol-5-yl)-1,4-dioxa-8-aza-spiro[4.5]decane | HCID 58397982 | — |
反応手順
To a prestirred solution (10 minutes at room temperature) of palladium(II) acetate (180 mg, 0.001 mmol) and 2-(dicyclohexylphosphino)biphenyl (572 mg, 0.002 mmol) in dioxane (10 mL) were added 1,4-dioxa-8-azaspiro(4,5)decane (1.3 mL, 10 mmol), 5-chloro-3-methyl-[1,2,4]thiadiazole (1.48 g, 11 mmol) and sodium tert-butylate (1.47 g, 15 mmol) and heated in the microwave at 130° C. for 15 minutes. The reaction mixture was diluted with half saturated brine, the aqueous phase was extracted with ethyl acetate, the combined organic phases were dried over sodium sulfate, the solvent was evaporated and the residue was purified by silica gel chromatography using ethyl acetate as eluent. The title compound was obtained as a light yellow solid (1.87 g, 77%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08486967B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-7ccbc31a04fd4186be31720467f31f27 |
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| 出典メモ | uspto-grants-2013_07 |
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