Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → (2,2-Dimethyl-5-oxo-[1,3]dioxolan-4-ylidene)-acetic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| 반응물 | (Z)-2,2-Dimethyl-5-(tert-butyldiphenylsilyloxycarbonyl-methylene)-1,3-dioxolan-4-one | HCID 21947558 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | (2,2-Dimethyl-5-oxo-[1,3]dioxolan-4-ylidene)-acetic acid | HCID 68860642 | 95% |
반응 단계
A solution of the crude (Z)-2,2-dimethyl-5-(tert-butyldiphenylsilyloxycarbonyl methylene)-1,3-dioxolan-4-one (52.4 mmol) in tetrahydrofuran (200 ml) was treated with acetic acid (13 ml) followed with 50 ml of a 1 M solution of tetrabutylammonium fluoride in tetrahydrofuran. After 15 minutes at 22° C., the reaction mixture was filtered and the filtrate was concentrated in vacuo. Trituration of the residue with toluene gave 6.3 g (70% yield for three steps) of the title material as a white solid (>95% pure by 1HNMR).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06777440B2 |
| 출처 데이터셋 | uspto-grants-2004_08 |
| ORD ID | ord-53b79126d86c4e3fbeec37a042280bae |
| 출처 메모 | uspto-grants-2004_08 |