関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | tert-Butyl 2,8-diazaspiro[4.5]decane-2-carboxylate | HCID 34178604 | — |
| 反応物 | 2,4-Dichlorofuro[3,2-D]pyrimidine | HCID 45789968 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Tert-butyl 8-(2-chlorofuro[3,2-d]pyrimidin-4-yl)-2,8-diazaspiro[4.5]decane-2-carboxylate | HCID 86665112 | 93.6% |
反応手順
A mixture of tert-butyl 2,8-diazaspiro[4.5]decane-2-carboxylate (0.83 g, 3.4 mmol, Alfa Aesar), 2,4-dichlorofuro[3,2-d]pyrimidine (0.65 g, 3.4 mmol, ArkPharm) and TEA (0.96 mL, 6.9 mmol) in 1,4-dioxane (35 mL) was stirred at about 25° C. for about 12 h. Water (4 mL) and EtOAc (25 mL) were added and the layers were separated. The organic layer was concentrated under reduced pressure to give tert-butyl 8-(2-chlorofuro[3,2-d]pyrimidin-4-yl)-2,8-diazaspiro[4.5]decane-2-carboxylate (1.25 g, 55%): LC/MS (Table 2, Method f) Rt=2.12 min; MS m/z: 393 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08551981B2 |
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| 出典データセット | uspto-grants-2013_10 |
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| ORD ID | ord-f8362b8cd12a4588ab303eac133a9ada |
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| 出典メモ | uspto-grants-2013_10 |
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