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 | 2,5-Dichloropyrimidine | HCID 590641 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 8-(5-Chloropyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4.5]decane | HCID 68290179 | — |
反応手順
1,4-Dioxa-8-azaspiro[4.5]decane (2.39 g) is combined with 2,5-dichloropyrimidine (2.44 g) in N,N-dimethylformamide (50 mL), 1,4-dioxane (75 mL) and triethylamine (6.7 mL) in a glass pressure reaction vessel. The mixture is heated with stirring at 120° C. for 16 h. After cooling to room temperature, the solution is concentrated and partitioned between dichloromethane (100 mL) and water (100 mL). The aqueous layer is extracted with dichloromethane (100 mL). The dichloromethane layers are combined, washed with water (2×100 mL), dried over Na2SO4, filtered and concentrated to yield the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822471B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-9a58d179ff614bf0bd54c20ea26b7417 |
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| 出典メモ | uspto-grants-2014_09 |
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