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Ethyl formate → Benzyl 2-chloro-3-oxopropanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl formate | HCID 8025 | — |
| 反応物 | Acetic acid, 2-chloro-, phenylmethyl ester | HCID 8786 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Benzyl 2-chloro-3-oxopropanoate | HCID 86672210 | — |
反応手順
To potassium tert-butoxide (141 mL, 141 mmol) at 0° C. was added dropwise a solution of benzyl 2-chloroacetate (26.8 g, 141 mmol) and ethyl formate (11.6 mL, 141 mmol) in Et2O (45 mL). The reaction was warmed to ambient temperature and stirred for 16 hours. The reaction mixture was filtered and washed with cold ether (100 mL). The potassium salt was dissolved in H2O (50 mL) and the solution was acidified with concentrated HCl to pH=4 in a cold bath. The solution was extracted with ether and the organic phase was dried (MgSO4) and concentrated to give the crude product. A lower boiling point impurity was removed by vacuum distillation (90° C., 5 mm Hg) and the residue was taken directly to the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08841455B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-cd736840933d49b08d4e6330be5fe87d |
| 出典メモ | uspto-grants-2014_09 |