Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl Acetate → 5-(Tert-butyldiphenylsilanyloxy)-3-(4-trifluoromethylphenyl)-pentanenitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Methyl dichlorophosphate | HCID 69611 | — |
| 반응물 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 반응물 | 5-(Tert-butyldiphenylsilanyloxy)-3-(4-trifluoromethylphenyl)pentanoic acid amide | HCID 66630138 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Heptane | HCID 8900 | — |
| 생성물 | 5-(Tert-butyldiphenylsilanyloxy)-3-(4-trifluoromethylphenyl)-pentanenitrile | HCID 66778011 | 97.3% |
반응 단계
5-(tert-Butyldiphenylsilanyloxy)-3-(4-trifluoromethylphenyl)pentanoic acid amide (640 mg) was dissolved in methylene chloride (13 mL), and 1,8-diazabicyclo[5,4,0]undec-7-ene (862 μL) and methyl dichlorophosphate (301 μL) were added at 0° C. After stirring at room temperature for 1.5 hours, the reaction was terminated with a saturated sodium bicarbonate aqueous solution. The organic layer was washed with brine and then dried over magnesium sulfate. Concentration under reduced pressure gave an oil. The oil was allowed to pass through a silica gel pad (mobile phase:ethyl acetate:heptane=1:2) to obtain the title compound (600 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08754100B2 |
| 출처 데이터셋 | uspto-grants-2014_06 |
| ORD ID | ord-0c8a6ef0d45e484282c68aa172cda9a4 |
| 출처 메모 | uspto-grants-2014_06 |