참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | N-Cyclohexyl-2-pyrrolidone | HCID 81278 | — |
| 반응물 | Lithium diisopropylamide | HCID 2724682 | — |
| 반응물 | 2-(Bromomethyl)-1,3-dichloro-5-methoxybenzene | HCID 59299479 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-Cyclohexyl-3-(2,6-dichloro-4-methoxy-benzyl)-pyrrolidin-2-one | HCID 59299414 | 69% |
반응 단계
Dissolve commercially available 1-cyclohexyl-pyrrolidin-2-one (88.2 g, 527.9 mmol) in 2500 mL tetrahydrofuran and cool to −78° C. Add 176 mL 2 M LDA and stir for ˜5 min. Add 2-bromomethyl-1,3-dichloro-5-methoxy-benzene (95 g, 351.9 mmol) and allow the reaction to warm to room temperature. Pour the mixture into saturated ammonium chloride and extract twice with dichloromethane. Dry over sodium sulfate, filter and concentrate under vacuum to obtain a tan solid. Add hexanes and stir rapidly before filtering. Wash the filter cake several times with cold hexane to obtain 86 g (69%) of a light-tan solid: MS (m/z): 356 (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-671ed090c526489ea143d527e9a47bc2 |
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| 출처 메모 | uspto-grants-2012_01 |
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