참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Chloride | HCID 5234 | — |
| 반응물 | Butylate | HCID 16181 | — |
| 반응물 | Potassium | HCID 5462222 | — |
| 반응물 | 4-(1,4-Dioxaspiro[4,5]dec-8-yl)-1-(3-fluorophenyl)-cyclohexane | HCID 21308588 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | HCID 178505689 | HCID 178505689 | 97.3% |
반응 단계
23.7 g of potassium t.-butylate were added to a solution of 125.3 g of 4-(1,4-dioxaspiro[4,5]dec-8-yl)-1-(3-fluorophenyl)-cyclohexane (cis/trans 50/47) in 630 ml of dimethyl sulphoxide, the mixture was stirred at 100° C. for 2 hrs., cooled and poured into 2500 ml of 5 percent sodium chloride solution. The reaction mixture was extracted with methylene chloride, the organic phase was dried over sodium sulfate, filtered and the filtrate was evaporated. Crystallization of the residue from isopropanol gave 121.9 g of trans-4-(1,4-dioxaspiro[4,5]dec-8-yl)-1-(3-fluorophenyl)cyclohexane as colorless crystals (trans content 99.8%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05888423 |
|---|
| 출처 데이터셋 | uspto-grants-1999_03 |
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| ORD ID | ord-5ec8769642e9475c888caa24dee08499 |
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| 출처 메모 | uspto-grants-1999_03 |
|---|