Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,2,7,7-Tetramethyl-3,6-dioxa-2,7-disilaoctane → 2-(2,2-Dimethyl-3-nitropropyl)-2-methyl-[1,3]dioxolane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,2,7,7-Tetramethyl-3,6-dioxa-2,7-disilaoctane | HCID 81858 | — |
| 반응물 | 4,4-Dimethyl-5-nitropentan-2-one | HCID 4156383 | — |
| 촉매 | Trimethylsilyl triflate | HCID 65367 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-(2,2-Dimethyl-3-nitropropyl)-2-methyl-[1,3]dioxolane | HCID 14638051 | 97.2% |
반응 단계
A stirred solution of 1,2-bis(trimethylsilyloxy)ethane (26.5 g, 128 mmol) in dichloromethane (50 mL) was cooled in a dry ice/isopropanol bath, and trimethylsilyl trifluoromethanesulfonate (2.2 g, 1.0 mmol) was added, followed by the dichloromethane solution of 4,4-dimethyl-5-nitropentan-2-one (50 mL, 19.0 g, 119 mmol) from the previous step. After 30 minutes, the cooling bath was removed and the solution was allowed to warm to room temperature. The solution was filtered through a plug of potassium carbonate and concentrated under reduced pressure to provide 2-(2,2-dimethyl-3-nitropropyl)-2-methyl-[1,3]dioxolane (23.5 g) as a dark oil that was used directly in the next step without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09328110B2 |
| 출처 데이터셋 | uspto-grants-2016_05 |
| ORD ID | ord-cc8b8aaf51d44583aafc7dd54d21a15e |
| 출처 메모 | uspto-grants-2016_05 |