참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Cyclopropyl methyl ketone | HCID 13004 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Ethyl 4-(methylsulphenyl)benzoate | HCID 10130363 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 3-Cyclopropyl-1-[4-(methylsulphenyl)-phenyl]-propan-1,3-dione | HCID 19931781 | 49.4% |
반응 단계
Cyclopropyl methyl ketone (0.84 g) was added to a suspension of sodium hydride (80%, 0.3 g) in dioxane. The mixture was stirred for 20 minutes and ethyl 4-(methylsulphenyl)benzoate (1.0 g) was added. The mixture was stirred and heated at 45° C. for 1.5 hours and at 60° C. for 2 hours. It was left to stand at room temperature overnight. Hydrochloric acid (2M) was added and the mixture was extracted with ethyl acetate, washed with water, dried (MgSO4) and filtered. The flitrate was evaporated to dryness and the residue was purified by chromatography eluted with a mixture of ethyl acetate and hexane to give 3-cyclopropyl-1-[4-(methylsulphenyl)-phenyl]-propan-1,3-dione (0.59 g) as an orange solid, NMR (CDCl3) 1.0(m,2H), 1.2(m,2H), 1.8(m, 1H), 2.5(s,3H), 6.25(s,1H), 7.25(d,2H), 7.8(d,2H), 16.35(bs,1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05424276 |
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| 출처 데이터셋 | uspto-grants-1995_06 |
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| ORD ID | ord-ff81f5e3b81e4e9384c51fa1f0552849 |
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| 출처 메모 | uspto-grants-1995_06 |
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