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Triethylamine → (R)-Methyl 2-(5-bromo-1-oxoisoindolin-2-yl)-3-methylbutanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methyl D-valinate hydrochloride | HCID 11984198 | — |
| 反応物 | Methyl 4-bromo-2-(bromomethyl)benzoate | HCID 22031079 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (R)-Methyl 2-(5-bromo-1-oxoisoindolin-2-yl)-3-methylbutanoate | HCID 86673568 | — |
反応手順
Methyl 4-bromo-2-(bromomethyl)benzoate (650 mg, 2.12 mmol) and D-valine methyl ester hydrochloride (527 mg, 3.15 mmol) was taken in toluene (6.5 mL) and to this reaction mixture, triethyl amine (428 mg, 4.24 mmol) was added and refluxed for about 16 h. After completion of the reaction, the reaction mixture was diluted with ethyl acetate and washed with water and brine, dried over anhydrous sodium sulfate and concentrated to obtain an oil, which was purified by column chromatography (silica gel, 30% ethyl acetate in petroleum ether) to obtain the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08748426B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-efc7154324b44a98a9ea05ea0f974348 |
| 出典メモ | uspto-grants-2014_06 |