Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 416015생성일: 2026년 10월 24일
Methyl iodide → 4-[3',5'-Dichloro-4'-(1-cyclohexyl-2-oxo-pyrrolidin-3-ylmethyl)-biphenyl-4-carbonyl]-1-methyl-piperazin-2-one
https://huagongshe.com/ko/reaction/416015
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Acetone diethylether | HCID 21584533 | — |
| 반응물 | Racemic 1-cyclohexyl-3-[3,5-dichloro-4'-(hexahydro-pyrrolo[1,2-a]pyrazine-2-carbonyl)-biphenyl-4-ylmethyl]-pyrrolidin-2-on | HCID 57741511 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 4-[3',5'-Dichloro-4'-(1-cyclohexyl-2-oxo-pyrrolidin-3-ylmethyl)-biphenyl-4-carbonyl]-1-methyl-piperazin-2-one | HCID 57741571 | 32% |
반응 단계
Treat a solution of racemic 1-cyclohexyl-3-[3,5-dichloro-4′-(hexahydro-pyrrolo[1,2-a]pyrazine-2-carbonyl)-biphenyl-4-ylmethyl]-pyrrolidin-2-on (0.245 g, 0.46 mmol) in dimethylformamide (6 mL) with 60% sodium hydride (0.037 g, 0.93 mmol) and stir for 15 minutes at room temperature under a nitrogen atmosphere. Cool the reaction to 0° C., treat with iodomethane (0.25 g, 1.76 mmol) and then stir at room temperature for 16 hours under a nitrogen atmosphere. Quench the reaction with 1N hydrochloric acid, dilute with ethyl acetate and wash with water. Dry the organic layer with sodium sulfate and purify by silica gel chromatography using a gradient of 0 to 10% methanol in dichloromethane to afford product. Re-crystallize from acetone/diethyl ether to afford 81 mg (32%) of the title compound: MS (m/z) 542 (M+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08088776B2 |
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| 출처 데이터셋 | uspto-grants-2012_01 |
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| ORD ID | ord-a152e68b21f74bb2913a78960c34c72e |
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| 출처 메모 | uspto-grants-2012_01 |
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