참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 8-Phenyl-1,4-dioxa-8-azaspiro[4.5]decane | HCID 11470039 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-Phenyl-4-piperidinone | HCID 413009 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05891889 |
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| 출처 데이터셋 | uspto-grants-1999_04 |
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| ORD ID | ord-f7d70bf0c69f4a24b3898e5d37b4402d |
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| 출처 메모 | uspto-grants-1999_04 |
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