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Ethyl Acetate → 4-(5-Chloro-2-methyl-phenyl)-pyridin-3-ylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | N-[4-(5-chloro-2-methyl-phenyl)-pyridin-3-yl]-2,2-dimethyl-propionamide | HCID 70663288 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 4-(5-Chloro-2-methyl-phenyl)-pyridin-3-ylamine | HCID 70663365 | — |
反応手順
A solution of N-[4-(5-chloro-2-methyl-phenyl)-pyridin-3-yl]-2,2-dimethyl-propionamide (1 g, 3.3 mmol) in 3M aqueous HCl (50 mL) was stirred at 90° C. for 18 hours. The reaction mixture was poured on 200 mL 1M aqueous NaOH solution and 150 mL EtOAc. The layers were separated and the aqueous layer was extracted a second time with 150 mL EtOAc. The combined organic layers were washed with 150 mL brine, dried over MgSO4, filtered and concentrated under vacuum. Light brown viscous oil (720 mg, 99%). MS (ESI): m/z=219.068 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08987307B2 |
| 出典データセット | uspto-grants-2015_03 |
| ORD ID | ord-2f35d54c1af04d49ab672d4b138870de |
| 出典メモ | uspto-grants-2015_03 |