참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-chloro-N-methylacetamide | HCID 66773 | — |
| 반응물 | 1-Benzylpiperazine | HCID 75994 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-(4-Benzyl-piperazin-1-yl)-N-methyl-acetamide | HCID 36845230 | 83% |
반응 단계
A mixture of 1-benzyl-piperazine (1.0 g, 5.67 mmol), 2-chloro-N-methylacetamide (671.2 mg, 6.24 mmol, 1.1 eq.), and potassium carbonate (941 mg, 6.81 mmol, 1.2 eq.) in anhydrous THF (23 mL) was stirred at 60° C. under N2 for 18 h. The mixture was cooled to rt and poured into EtOAc. The organic phase was washed with water and brine, dried over Na2SO4, filtered, and concentrated in vacuo. The residue was purified by MPLC (Biotage®, gradient elution 1:4:5 v/v MeOH:Acetone:DCM) to give 1.16 g (83%) of the product as a white solid. 1H-NMR (300 MHz, DMSO-d6) 7.62 to 7.56 (broad d, 1H), 7.33 to 7.20 (m, 5H), 3.45 (s, 2H), 2.85 (s, 2H), 2.58 (d, 3H), 2.44 to 2.33 (broad s, 8H); ES-MS m/z 248.2 [M+H]+, RT (min) 0.33.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08431695B2 |
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| 출처 데이터셋 | uspto-grants-2013_04 |
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| ORD ID | ord-3cf0cccfa4de48788a451027f19e9182 |
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| 출처 메모 | uspto-grants-2013_04 |
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