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Water → Ethyl 3-(octahydroquinolin-1-yl)-3-oxopropionate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Decahydroquinoline | HCID 92911 | — |
| 反応物 | Ethyl 3-chloro-3-oxopropionate | HCID 118931 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl 3-(octahydroquinolin-1-yl)-3-oxopropionate | HCID 66794569 | 78.9% |
反応手順
3.38 mL of Et3N and 1.44 mL (11 mmol) of ethyl 3-chloro-3-oxopropionate are added to a solution of 1.5 mL (10 mmol) of decahydroquinoline in 100 mL of AcOEt. The resulting solution is kept under stirring at reflux for 10 h. Then water is added and the organic phase is separated, the aqueous phase is extracted once again with AcOEt. The organic phases are pooled and they are first washed with 5% solution of NaHCO3 and subsequently with brine, they are dried over anhydrous Na2SO4, they are filtered and the solvent is evaporated under reduced pressure. 2.0 g of a yellow oil are obtained. It is identified as intermediate IIIa.1. Method A: tr: 6.76 min; m/z: 268.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822452B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-e6a5c0325d5a4f4c8690b3127b1584ef |
| 出典メモ | uspto-grants-2014_09 |