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Ethyl chloroacetate → (2,2-Dimethyl-pyrrolidin-1-yl)-acetic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl chloroacetate | HCID 7751 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,2-Dimethylpyrrolidine | HCID 414773 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | (2,2-Dimethyl-pyrrolidin-1-yl)-acetic acid ethyl ester | HCID 63219360 | 61.5% |
反応手順
Ethylchloroacetate (0.15 ml, 1.37 mmol), potassium carbonate (416 mg, 1.5 mmol) and 2,2-dimethyl-pyrolidine (0.280 mg, 2.06 mmol) were suspended in ethanol (3 ml) and subjected to microwave irradiation at 120° C. for 45 min. The resultant mixture was suspended in diethyl ether (30 ml), extracted with 2M hydrochloric acid (30 ml) and the organic layer discarded. The aqueous layer was treated with a slight excess of 4N sodium hydroxide solution and extracted with diethyl ether (3×30 ml). The organic layers were combined, dried over sodium sulfate, filtered and solvent removed under reduced pressure to afford (2,2-dimethyl-pyrrolidin-1-yl)-acetic acid ethyl ester (156 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07700634B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-7bfcbf497a894ea8867f2117c7808ace |
| 出典メモ | uspto-grants-2010_04 |