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Lithium borohydride → 7-Hydroxymethyl-6,7-dihydrodibenzo[c,e]azepin-5-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium borohydride | HCID 4148881 | — |
| 反応物 | 7-Oxo-6,7-dihydro-5H-dibenzo[c,e]azepine-5-carboxylic Acid Methyl Ester | HCID 68838469 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 7-Hydroxymethyl-6,7-dihydrodibenzo[c,e]azepin-5-one | HCID 68842223 | — |
反応手順
To a solution of 7-oxo-6,7-dihydro-5H-dibenzo[c,e]azepine-5-carboxylic acid methyl ester (120 mg, 0.45 mmol) in MeOH (5 mL) at 0° C. is added LiBH4 (20 mg, 0.9 mmol). The mixture is allowed to warm to RT and stirred there for 18 h. Additional LiBH4 is added until starting material is consumed. The solvent is removed under reduced pressure and water is added. The mixture is extracted with EtOAc and the organic phase is washed with brine and dried over magnesium sulfate. The solvent is removed under reduced pressure to give the title compound which is used directly in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08084448B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-f34b84d44a934cc78da113115b2f44ba |
| 出典メモ | uspto-grants-2011_12 |