化工社化工社 化学情報印刷レポート · 研究参考用
Dibenz(b,f)azepine → (Z)-methyl 4-((5H-dibenzo[b,f]azepin-5-yl)methyl)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dibenz(b,f)azepine | HCID 9212 | — |
| 反応物 | Dibutyltin dichloride | HCID 12688 | — |
| 反応物 | Phenylsilane | HCID 12752 | — |
| 反応物 | Methyl 4-Formylbenzoate | HCID 15294 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (Z)-methyl 4-((5H-dibenzo[b,f]azepin-5-yl)methyl)benzoate | HCID 59783517 | 83% |
反応手順
(Z)-5H-Dibenzo[b,f]azepine (100 mg, 0.52 mmol), dibutyltin dichloride (54 mg, 0.16 mmol) and methyl 4-formylbenzoate (260 mg, 1.60 mmol) were stirred in THF (2 mL) for 30 minutes. Phenylsilane was added and the reaction mixture was stirred for 3 days. The solvent was evaporated and the residue was purified by flash chromatography (0% to 40% EtOAc in hexanes). The fractions containing some product were washed with Na2S2O4. The layers were split and the organic layer was evaporated to afford title compound 350 (147 mg, 83%) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09193749B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-7abb1a6f4fef4ff6bddca28cd544f8f0 |
| 出典メモ | uspto-grants-2015_11 |