化工社化工社 化学情報印刷レポート · 研究参考用
Hydrogen Peroxide → Tert-butyl 3-oxo-2-oxa-8-azaspiro[4.5]decane-8-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium Thiosulfate Pentahydrate | HCID 61475 | — |
| 反応物 | Tert-butyl 2-oxo-7-azaspiro[3.5]nonane-7-carboxylate | HCID 11195798 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Tert-butyl 3-oxo-2-oxa-8-azaspiro[4.5]decane-8-carboxylate | HCID 22744536 | — |
反応手順
567 ml solution of 37.8 g tert-butyl 2-oxo-7-azaspiro[3.5]nonane-7-carboxylate in methanol was cooled on ice water, and 43 g of 30% aqueous hydrogen peroxide was added dropwise thereinto. 63 ml of 1 N aqueous sodium hydroxide was added dropwise thereto, and the mixture was stirred at room temperature for 2 hr. 1000 ml ethyl acetate, 600 ml water and 100 ml saturated aqueous sodium thiosulfate pentahydrate were added thereto, and the organic layer was recovered. The extracted solution was washed with brine, dried over anhydrous magnesium sulfate, and then filtered. The filtrate was evaporated to give 28.4 g of tert-butyl 3-oxo-2-oxa-8-azaspiro[4.5]decane-8-carboxylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06699870B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-a505a4a908504f4f8d513ef2b414c003 |
| 出典メモ | uspto-grants-2004_03 |