참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Iodide | HCID 4875 | — |
| 반응물 | Methyl Chloride | HCID 6327 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 2-Methyl-5-(4-chlorobenzylidene)-cyclopentanone | HCID 53752951 | — |
| 용매 | tert-Butanol | HCID 6386 | — |
| 생성물 | 5-[(4-Chlorophenyl)methylidene]-2,2-dimethylcyclopentan-1-one | HCID 53421021 | 100.1% |
반응 단계
106 g of 2-methyl-5-(4-chlorobenzylidene)-cyclopentanone, 49.5 g of 85% strength aqueous potassium hydroxide solution, 8.3 g of potassium iodide and 400 g of tert-butanol were weighed in succession into a 700 ml stainless steel autoclave, and 50.5 g of methyl chloride were injected at 20° C. The mixture was stirred at room temperature for 23 hours and then 300 ml of tert-butanol were distilled off at 20 mbar up to an overhead temperature of max. 50° C. 400 ml of water were added to the residue, and the mixture was stirred thoroughly. The resulting suspension was filtered off over a suction filter, and the filter cake was washed twice with 200 ml of water each time and dried. 112.8 g of a pale beige solid were thus obtained with a purity of 89.5%. The yield of the crude product was 90.2% of theory.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05663447 |
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| 출처 데이터셋 | uspto-grants-1997_09 |
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| ORD ID | ord-81f1c423030e48d895584eec98bf4d1e |
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| 출처 메모 | uspto-grants-1997_09 |
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