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Hydrochloric Acid → 3-Ethyl-8-benzyl-1-oxa-3,8-diazaspiro[4.5]decan-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-Oxa-3,8-diazaspiro(4.5)decan-2-one, 8-benzyl- | HCID 199815 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Ethyl-8-benzyl-1-oxa-3,8-diazaspiro[4.5]decan-2-one | HCID 13016590 | — |
反応手順
A mixture of 16.5 g 8-benzyl-1-oxa-3,8-diazaspiro[4.5]decan-2-one, 6.6 g, 50% suspension of sodium hydride in mineral oil, 15 g ethyl iodide and 70 ml N,N-dimethylformamide is heated at 90° for one hour. The mixture is poured into 150 ml water and the resulting mixture acidified with 10 N hydrochloric acid. The mixture is extracted with two 100 ml portions of hexane. The aqueous layer is basified with sodium hydroxide and extracted with three 75 ml portions of dichloromethane. Removal of solvent in vacuum affords a residue which when crystallized from heptane gives 3-ethyl-8-benzyl-1-oxa-3,8-diazaspiro[4.5]decan-2-one, mp 105°-106°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04255432 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-9e9fd3dfb19e4dd4a035093bee46bbdc |
| 出典メモ | uspto-grants-1981_03 |