참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Benzoyl chloride, 3-bromo- | HCID 74377 | — |
| 반응물 | 3-Buten-2-one, 4-methoxy- | HCID 94297 | — |
| 반응물 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | (E)-1-(3-Bromo-phenyl)-5-methoxy-pent-4-ene-1,3-dione | HCID 67318718 | — |
반응 단계
In a 1 ltr flask is cooled a solution of lithium hexamethyldisilazide (65 ml, 1.5 M) in THF (250 ml) to 75 ° C. During a period of 1 h is added 4-methoxy-but-3-en-2-one (7 ml). The mixture is stirred for 1 h at −70° C. A solution of 3-bromobenzoylchloride (6 g) in THF (250 ml) is added to the above mixture during 1 h at −70° C. The resulting mixture is slowly heated to ambient temperature and stirred for 1 h. Subsequently, the mixture is added to a cold aqueous solution of ammonium chloride and the resulting suspension is extracted with ethyl acetate. The organic phase is extracted twice with an aqueous solution of ammonium chloride, dried over sodium sulfate and evaporated. The crude oily product is transferred to the next step without any further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07745446B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-99ee562778c24210ad8e6056e2283f5e |
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| 출처 메모 | uspto-grants-2010_06 |
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