関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Cyanopiperidine | HCID 138223 | — |
| 反応物 | 2,4-Dichlorofuro[3,2-D]pyrimidine | HCID 45789968 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-(2-Chlorofuro[3,2-d]pyrimidin-4-yl)piperidine-4-carbonitrile | HCID 86665110 | 90.6% |
反応手順
A mixture of 2,4-dichlorofuro[3,2-d]pyrimidine (0.40 g, 2.1 mmol, ArkPharm), piperidine-4-carbonitrile (0.23 g, 2.1 mmol, Oakwood) and TEA (0.59 mL, 4.2 mmol) in 1,4-dioxane (10 mL) was stirred at about 25° C. for about 12 h. The solvent was removed under reduced pressure and water (5 mL) and DCM (10 mL) were added to the residue. The layers were separated and the organic solution was concentrated under reduced pressure to give 1-(2-chlorofuro[3,2-d]pyrimidin-4-yl)piperidine-4-carbonitrile (0.50 g, 90%): LC/MS (Table 2, Method 1) Rt=0.76 min; MS m/z: 263 (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-f1b6dfa90d5b464cab405f3abfa1d06a |
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| 出典メモ | uspto-grants-2013_10 |
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