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Water → Ethyl {[2-(1,3-benzodioxol-5-yl)-2-oxoethyl]thio}acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl Thioglycolate | HCID 12185 | — |
| 反応物 | 1-(1,3-Dioxaindan-5-yl)-2-bromoethan-1-one | HCID 243777 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Ethyl {[2-(1,3-benzodioxol-5-yl)-2-oxoethyl]thio}acetate | HCID 43218502 | — |
反応手順
Ethyl 2-mercaptoacetate (9.68 mL, 88.3 mmol) was added dropwise to a suspension of K2CO3 (12.2 g, 88.3 mmol) and 1-(1,3-benzodioxol-5-yl)-2-bromoethanone (21.4 g, 88.3 mmol) in dry acetone (100 mL). The mixture was stirred at reflux for seven hours, cooled at an icebath and added 200 mL water. Diethyl ether (400 mL) was added and the phases were separated. The aqueous layer was extracted with diethyl ether (200 mL) and the combined organic layers were washed with brine (200 mL), dried (MgSO4) and concentrated. This afforded the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07906502B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-00a960acb4124e9db5ade53abf3de7aa |
| 出典メモ | uspto-grants-2011_03 |