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Potassium Carbonate → 6-benzylamino-3,4-dihydro-2H-isoquinolin-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 6-Fluoro-1,2,3,4-tetrahydroisoquinolin-1-one | HCID 10725709 | — |
| 溶媒 | Benzylamine | HCID 7504 | — |
| 生成物 | 6-benzylamino-3,4-dihydro-2H-isoquinolin-1-one | HCID 67223915 | 35% |
反応手順
A solution of 6-fluoro-3,4-dihydro-2H-isoquinolin-1-one (300 mg, 1.81 mmol) and potassium carbonate (550 mg, 3.98 mmol) in benzylamine (1.5 ml) was stirred at 180° C. in a microwave for 2 hrs. The solvent was evaporated and the resulting residue partitioned between ethyl acetate (10 ml) and water (10 ml). The organic phase was separated, washed with brine (10 ml), then dried (MgSO4) and evaporated in vacuo. The crude residue was purified by preparative HPLC (Method A) to yield the title compound as a colourless solid (80 mg, 18%). HPLC retention time 3.81 min. Mass spectrum (ES+) m/z 253 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08399481B2 |
| 出典データセット | uspto-grants-2013_03 |
| ORD ID | ord-fa7e5e71fe5642d8a90aa87b2e5ae477 |
| 出典メモ | uspto-grants-2013_03 |