関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 8-Phenyl-1,4-dioxa-8-azaspiro[4.5]decane | HCID 11470039 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Phenyl-4-piperidinone | HCID 413009 | — |
反応手順
8-Phenyl-1,4-dioxa-8-azaspiro[4.5]decane (18.1 g, 82.5 mmol) was dissolved in a mixture of acetic acid (150 mL), water (150 mL), and conc. hydrochloric acid (38 mL) and the resulting solution was heated to 50° C. for 18 hrs. The reaction mixture was cooled in an ice-water bath, and sodium hydroxide pellets were added in portions until the mixture was neutralized. This mixture was extracted with dichloromethane (3×300 mL) and the combined organic extracts were dried over MgSO4, filtered, and concentrated in vacuo to give a dark oil. Chromatography on silica gel, eluting with hexane--10% ethyl acetate gave the product as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05891889 |
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| 出典データセット | uspto-grants-1999_04 |
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| ORD ID | ord-f7d70bf0c69f4a24b3898e5d37b4402d |
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| 出典メモ | uspto-grants-1999_04 |
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