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Water → {1-[4-(4-Fluoro-phenyl)phthalazin-1-yl]piperidin-4-yl}-methyl-carbamic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Chloro-4-(4-fluorophenyl)phthalazine | HCID 2115239 | — |
| 反応物 | 4-N-Boc-4-N-Methyl-aminopiperidine | HCID 2756806 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | {1-[4-(4-Fluoro-phenyl)phthalazin-1-yl]piperidin-4-yl}-methyl-carbamic acid tert-butyl ester | HCID 58157128 | 95.1% |
反応手順
Combine methyl-piperidin-4-yl-carbamic acid tert-butyl ester (75 g, 349 mmol), 1-chloro-4-(4-fluoro-phenyl)-phthalazine (75 g, 289 mmol), and potassium carbonate (80 g, 579 mmol) in dimethyl sulfoxide (500 mL) and heat the mixture to 110° C. for 3 h. Cool the reaction to ambient temperature and pour the slurry into water (1.0 L). Collect the solids by filtration and dry in a vacuum oven for 3 days to provide the title compound as a white solid (120 g, 95%). ES/MS m/z 437.3 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07981892B2 |
| 出典データセット | uspto-grants-2011_07 |
| ORD ID | ord-52d5ae3a476f4396aa21aac3175b0b4d |
| 出典メモ | uspto-grants-2011_07 |