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Methyl chloroformate → 2-(3-Methoxycarbonylamino-2-oxo-piperidin-1-yl)-propionic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl chloroformate | HCID 6586 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | 2-(3-Amino-2-oxo-piperidin-1-yl)-propionic acid ethyl ester | HCID 64237918 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(3-Methoxycarbonylamino-2-oxo-piperidin-1-yl)-propionic acid ethyl ester | HCID 66620164 | 75% |
反応手順
Methyl chloroformate (192 μL, 2.5 mmol) was added to a solution of 2-(3-amino-2-oxo-piperidin-1-yl)-propionic acid ethyl ester (353 mg, 1.6 mmol) and 4-methylmorpholine (907 μL, 8.24 mmol) in dichloromethane (10 mL). After 15 minutes the mixture was diluted with dichloromethane (20 mL) and washed with water (10 mL), and aqueous hydrogen chloride (0.5 N, 10 mL). The organic phase was dried over sodium sulfate and filtered. The solvent was removed under reduced pressure to provide 2-(3-methoxycarbonylamino-2-oxo-piperidin-1-yl)-propionic acid ethyl ester (332 mg, 1.2 mmol, 75%). C12H20N2O5 calculated 272.1 observed [M+1]+273.0; rt=1.82 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08088368B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-4a69930c61b14c24a4534d7bddb50ec3 |
| 出典メモ | uspto-grants-2012_01 |