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Hydrochloric Acid → 4-phenyl-N-(piperidine-4-yl)quinazolin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Amino-1-Boc-piperidine | HCID 1268291 | — |
| 反応物 | 2-Chloro-4-phenylquinazoline | HCID 3123582 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-phenyl-N-(piperidine-4-yl)quinazolin-2-amine | HCID 44140438 | 117.1% |
反応手順
A solution of 2-chloro-4-phenylquinazoline (1.38 g, 5.75 mmol), and tert-butyl 4-aminopiperidine-1-carboxylate (2.81 g, 14.1 mmol) was heated at reflux in n-butanol (20 mL) for 4 h. After removal of the n-butanol on a rotary evaporator, dichloromethane (100 mL) was added and the suspension was sonicated for 30 min and filtered. The solution was then concentrated on a rotary evaporator to give a brown residue. This residue was purified by column chromatography on silica gel (95:5 hexanes/ethyl acetate) to yield a green oil that was treated with 4M HCl in 1,4-dioxane (100 mL) at 100° C. for 1 h. The solvent was removed on a rotary evaporator to give 4-phenyl-N-(piperidine-4-yl)quinazolin-2-amine (2.05 g, 90%) as a dark yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08222263B2 |
| 出典データセット | uspto-grants-2012_07 |
| ORD ID | ord-4693dc3adecb40f5a3bd26120cc7b6dd |
| 出典メモ | uspto-grants-2012_07 |