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Benzyl chloroformate → (S)-2-Benzyloxycarbonylamino-3-(4-hydroxy-phenyl)-2-methyl-propionic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzyl chloroformate | HCID 10387 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | (S)-Methyl 2-amino-3-(4-hydroxyphenyl)-2-methylpropanoate hydrochloride | HCID 24847455 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (S)-2-Benzyloxycarbonylamino-3-(4-hydroxy-phenyl)-2-methyl-propionic acid methyl ester | HCID 66719336 | — |
反応手順
To a suspension of (S)-2-amino-3-(4-hydroxy-phenyl)-2-methyl-propionic acid methyl ester hydrochloride in ethyl acetate (25 mL) was added 1N NaHCO3 solution (12.5 ml.) and the mixture was stirred rapidly at ambient temperature for the addition of neat benzyl chloroformate (0.859 g, 1.01 eq., 5.05 mmol). Following addition, the reaction mixture was stirred for an additional hour; TLC and LC-MS analysis showed the reaction to be complete. The mixture was partitioned and the organic phase was separated and dried over Na2SO4 and concentrated. The crude product was used directly in the subsequent reaction without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07727983B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-453b935c31c044258a78e94583fc8b0d |
| 出典メモ | uspto-grants-2010_06 |