関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Bromovaleryl chloride | HCID 521173 | — |
| 反応物 | 4-Amino-7-(trifluoromethyl)quinoline | HCID 2735960 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 5-Bromo-N-(7-(trifluoromethyl)quinolin-4-yl)pentanamide | HCID 57629423 | 90% |
反応手順
4-Amino-7-trifluoromethylquinoline (120 mg, 0.56 mmol), triethylamine (170 mg, 1.7 mmol) and CHCl3 (4 mL) were charged in a 10 ml round-bottomed flask equipped with a magnetic stirrer. 5-Bromovaleryl chloride (140 mg, 0.7 mmol in CHCl3 (2 mL) were added and the reaction mixture was stirred for 15 h at 20° C. The reaction mixture was poured in 10 mL of H2O and extracted with CH2Cl2 (100 mL). The organic layer was washed with brine (2×10 mL), dried over MgSO4, filtered and evaporated at 30° C. to dryness. The crude compound was purified by column chromatography (SiO2; CH2Cl2:MeOH=99.5:0.5 to 98:2) to give after evaporation 5-bromo-N-(7-(trifluoromethyl)quinolin-4-yl)pentanamide 32 (190 mg, 90% yield) as a beige solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07514432B2 |
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| 出典データセット | uspto-grants-2009_04 |
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| ORD ID | ord-f75ee1d4f13044f584c5438a19a7d8f4 |
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| 出典メモ | uspto-grants-2009_04 |
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