참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | alpha-Methylbutyrolactone | HCID 98323 | — |
| 반응물 | 4-Benzylpiperazin-1-amine | HCID 12198453 | — |
| 촉매 | Zincchloride | HCID 3007855 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(4-Benzylpiperazin-1-yl)-3-methylpyrrolidin-2-one | HCID 68417748 | 37% |
반응 단계
A mixture of 3-methyldihydrofuran-2(3H)-one (2.0 g), thionyl chloride (1.5 ml) and zinc chloride (10 mg) was stirred at 80° C. for 15 hours. The mixture was cooled to room temperature, and the reaction mixture was added dropwise to a solution of 4-benzylpiperazin-1-amine (3.8 g) in THF (50 mL) at 0° C., followed by stirring at 0° C. for 2 hours. Sodium hydride (60% in oil; 2.4 g) was added thereto and the mixture was stirred at room temperature for 15 hours. Ice was added thereto, and then the reaction mixture was concentrated under reduced pressure. The residue was diluted with water, and extracted with dichloromethane. The extract was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue obtained was purified by basic silica gel column chromatography (ethyl acetate/hexane=1/5) to obtain the title compound (2.0 g, 37%) as a yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07745623B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-7a115c64888a4ebcb4f269e186d5cbbd |
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| 출처 메모 | uspto-grants-2010_06 |
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