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Benzyl chloroformate → Ethyl 3-{[(benzyloxy)carbonyl]amino}propanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzyl chloroformate | HCID 10387 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | beta-Alanine, ethyl ester, hydrochloride | HCID 458475 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 3-{[(benzyloxy)carbonyl]amino}propanoate | HCID 12116647 | — |
反応手順
Ethyl 3-aminopropionate hydrochloride (10 g) was dissolved in a mixture of tetrahydrofuran (100 ml) and water, which was cooled at 0° to 5° C. in an ice bath and adjusted to pH 8.2 with 30% aqueous sodium hydroxide solution. To a resulting solution was added with care benzyloxycarbonyl chloride (10.3 ml), with maintaining the pH from pH 8.0 to 9.0 with 30% aqueous sodium hydroxide solution at 0° to 5° C. The reaction mixture was extracted with ethyl acetate (300 ml) and organic layer was separated, which was washed two times with saturated sodium chloride in water and dried over magnesium sulfate. Solvent was removed under reduced pressure to give ethyl 3-(benzyloxycarbonylamino)-propionate (15.3 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05773530 |
| 出典データセット | uspto-grants-1998_06 |
| ORD ID | ord-b5f446095697466692242d5efe51023c |
| 出典メモ | uspto-grants-1998_06 |