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Water → 4-Nitrophenyl 1-(4-(trifluoromethyl)phenyl)-3,4-dihydroisoquinoline-2(1H)-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4-Nitrophenyl chloroformate | HCID 82129 | — |
| 反応物 | 1-(4-(Trifluoromethyl)phenyl)-1,2,3,4-tetrahydroisoquinoline | HCID 16640696 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Nitrophenyl 1-(4-(trifluoromethyl)phenyl)-3,4-dihydroisoquinoline-2(1H)-carboxylate | HCID 42635102 | — |
反応手順
To a solution of 1-(4-(trifluoromethyl)phenyl)-1,2,3,4-tetrahydroisoquinoline (200 mg, 0.721 mmol, example 9 (step 3) and DIEA (126 μL, 0.721 mmol) in DCM (4 mL) was added 4-nitrophenyl chloroformate (145 mg, 0.721 mmol). The resulting mixture was stirred at RT for 16 h. Then, H2O (10 mL) was added and the mixture was extracted with DCM (2×5 mL). The combined organic extracts were dried over MgSO4 and concentrated. The residue was purified by silica gel flash column chromatography (0%-50% EtOAc/hexane) to give the title compound as a white oil. MS (ESI, positive ion) m/z: 443 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08476297B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-af957338c2bb4a96a53b585316e744ee |
| 出典メモ | uspto-grants-2013_07 |