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Methanol → Methyl 3-oxocyclohexane-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Trimethylsilyldiazomethane | HCID 167693 | — |
| 反応物 | 3-Oxocyclohexane-1-carboxylic acid | HCID 2760252 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Methyl 3-oxocyclohexane-1-carboxylate | HCID 566099 | — |
反応手順
To a solution of 3-oxocyclohexanecarboxylic acid (1.0 g, 7.0 mmol) in diethyl ether (28 mL) was added dropwise TMS-diazomethane (3.5 mL, 7.0 mmol, 2.0 mL in diethyl ether). MeOH (30 mL) was added and the mixture was maintained at ambient temperature for 30 minutes. The mixture was concentrated in vacuo, and the residue was purified by MPLC on silica gel (using a gradient elution of 0-45% EtOAc/hexanes). Desired fractions were identified, combined, and concentrated in vacuo to afford the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09328099B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-331e63e2801142b8af421c08c9574e82 |
| 出典メモ | uspto-grants-2016_05 |