関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-Methylaniline | HCID 7515 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 6-Bromo-1-tetralone | HCID 10105069 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 触媒 | Binap, (A+-)- | HCID 634876 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 6-[Methyl(phenyl)amino]-1,2,3,4-tetrahydronaphthalen-1-one | HCID 118597757 | 68% |
反応手順
To a solution of 6-bromo-1,2,3,4-tetrahydronaphthalen-1-one (2.0 g, 8.9 mmol) in toluene (20 mL) was added N-methylaniline (960 mg, 8.9 mmol), Cs2CO3 (4.4 g, 13.4 mmol), BINAP (310 mg, 0.5 mmol) and Pd(OAc)2 (110 mg, 0.5 mmol). The mixture was stirred overnight at 100° C. under nitrogen. The mixture was filtered and concentrated, and the residue was purified by silica gel chromatography (30%-80% EtOAc/Hex) to give 1.52 g (68%) of the title compound as a light brown oil. [M+H] calc'd for C17H17NO, 252. found 252.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09447046B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-1ff2332d81f540fa964a3c1b613116a1 |
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| 出典メモ | uspto-grants-2016_09 |
|---|
