関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-(2-Chloroethyl)pyrrolidine hydrochloride | HCID 81668 | — |
| 反応物 | Acetamide, N-(2-hydroxy-5-nitrophenyl)- | HCID 3292867 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(5-nitro-2-(2-(pyrrolidin-1-yl)ethoxy)phenyl)acetamide | HCID 58098809 | 33% |
反応手順
To a solution of N-(2-hydroxy-5-nitrophenyl)acetamide (870 mg, 4.44 mmol) in DMF (5 mL) was added NaH (196 mg, 5.32 mmol) and K2CO3 (2.11 g, 13.32 mmol), followed by 1-(2-chloroethyl)pyrrolidine hydrochloride (905 mg, 5.32 mmol). After heating at 100° C. for 20 h, the solution was poured to ice, and was extracted with EtOAc, organic layer was washed with Sat. NaHCO3, brine, dried and concentrated to give N-(5-nitro-2-(2-(pyrrolidin-1-yl)ethoxy)phenyl)acetamide (430 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08367689B2 |
|---|
| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-182f0f1697c64ecc978d4050f6b5f349 |
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| 出典メモ | uspto-grants-2013_02 |
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