참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Butanoic acid, 2-bromo-, ethyl ester | HCID 79039 | — |
| 반응물 | 4-Phenyl-delta-valerolactam | HCID 3279694 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | Ethyl 2-(2-oxo-5-phenyl-1-piperidinyl)butanoate | HCID 11358220 | 70.4% |
반응 단계
In a 1 l three necked flask fitted with reflux condenser, magnetic stirrer and dropping funnel under inert atmosphere, 9.8 g (87 mmoles) of potassium t-butoxide were suspended in 600 ml of dry toluene. 11.8 g (67 mmoles) of 5-phenyl-2-piperidinone 25 were added, and the mixture stirred for 30 min. 17 g (87 mmoles) of ethyl 2-bromobutanoate were added and the temperature raised to 70° C. for 5 hours. 600 ml of ethyl acetate were added, the solution was washed twice with brine, the organic phase dried over magnesium sulfate, filtered and concentrated to dryness. The residue was purified by PrepLC (1 kg SiO2, CH2Cl2/EtOH, 97.5/2.5) to give 3.7 g of pure ester 26 as a mixture of diastereomers, 70.4% yield.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07473697B2 |
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| 출처 데이터셋 | uspto-grants-2009_01 |
|---|
| ORD ID | ord-7dc173ddcfed4c0f8bed5da2a38e6045 |
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| 출처 메모 | uspto-grants-2009_01 |
|---|
