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Triethylamine → 3-[2-Benzyl-1-oxo-1,2-dihydroisoquinolin-6-yl]-acrolein
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Acrolein dimethyl acetal | HCID 80145 | — |
| 反応物 | Tri-o-tolylphosphine | HCID 80271 | — |
| 反応物 | 2-Benzyl-6-bromo-isoquinolin-1-one | HCID 18963984 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-[2-Benzyl-1-oxo-1,2-dihydroisoquinolin-6-yl]-acrolein | HCID 53919284 | — |
反応手順
A mixture of 2-benzyl-6-bromo-1,2-dihydro-1-oxoisoquinoline (1 g, 3.2 mmol), acrolein dimethyl acetal (2.6 mL, 22.4 mmol), Pd(OAc)2 (15 mg, 0.064 mmol), P(o-tolyl)3 (78 mg, 0.26 mmol) and Et3N (0.5 mL, 3.84 mmol) in DMF (2 mL) is heated in a sealed tube apparatus at 120° for 48 hours. After cooling to room temperature, the reaction mixture is diluted with EtOAc, filtered, washed with saturated NaCl solution, dried over MgSO4 concentrated in vacuo, and the residue is chromatographed (silica gel 1:4 EtOAc/hexane) to yield 3-[2-benzyl-1-oxo-1,2-dihydroisoquinolin-6-yl]-acrolein.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05334600 |
| 出典データセット | uspto-grants-1994_08 |
| ORD ID | ord-1b40f671cefb4b60846d5f217aea54db |
| 出典メモ | uspto-grants-1994_08 |