참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Methyl Ethyl Ketone | HCID 6569 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 3-Cyclopentene-1-acetaldehyde, 2,2,3-trimethyl- | HCID 98497 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 3-Penten-2-one, 3-methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)- | HCID 6436969 | 60.4% |
반응 단계
152 G (1.0 M) of campholenic aldehyde having a purity of about 75% were added dropwise under stirring in 15-20 minutes to a mixture cooled at -5/-10° of 400 g (6.1 M) of methyl-ethyl ketone, 1025 g (35 M) of methanol, 30.5 g (0.54 M) of potassium hydroxide and 380 g of water. The mixture was kept at -5° for 24 hours, then at room temperature for the same period and neutralized thereupon with H2SO4 to 62.5%. After concentration under reduced pressure, the obtained residue was dissolved in 200 ml of water, diluted with petrol ether 30/50, washed until neutrality, dried and concentrated. 189.3 G of a raw material was thus obtained which on distillation with a Vigreux column of 15 cm length gave 144.6 g of (E)-3-methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)-3-penten-2-one having a purity of 86% (yield 60.4%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04610813 |
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| 출처 데이터셋 | uspto-grants-1986_09 |
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| ORD ID | ord-2df230ea3a7f4123889382b5a88a7f02 |
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| 출처 메모 | uspto-grants-1986_09 |
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