Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
(Trifluoromethyl)trimethylsilane → 8-(2-Chloro-benzenesulfonyl)-2-[4-(2,2,2-trifluoro-1-hydroxy-1-methyl-ethyl)-phenyl]-2,8-diaza-spiro[4.5]decan-1-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | (Trifluoromethyl)trimethylsilane | HCID 552549 | — |
| 반응물 | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| 반응물 | 2-(4-Acetyl-phenyl)-8-(2-chloro-benzenesulfonyl)-2,8-diaza-spiro[4.5]decan-1-one | HCID 59577963 | — |
| 촉매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 8-(2-Chloro-benzenesulfonyl)-2-[4-(2,2,2-trifluoro-1-hydroxy-1-methyl-ethyl)-phenyl]-2,8-diaza-spiro[4.5]decan-1-one | HCID 59578032 | 60.5% |
반응 단계
2-(4-Acetyl-phenyl)-8-(2-chloro-benzenesulfonyl)-2,8-diaza-spiro[4.5]decan-1-one (0.13 g), product of example 151), dissolved in THF (12 ml) under an argon atmosphere was treated at RT with (trifluoromethyl)trimethylsilane (0.062 g) then with tetra-n-butylammonium fluoride (1M solution in THF, 0.29 ml) and the reaction mixture was stirred overnight at RT. The mixture was made acidic with 3M aqueous HCl (a few drops) and stirred further 15 minutes. The solvent was removed in vacuo and the residue adsorbed on silica gel and chromatographed over silica gel (AcOEt/heptane, gradient from 0 to 40%) to give the desired product as white solid (0.091 g). MS (ESI): 517.1 MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08329904B2 |
| 출처 데이터셋 | uspto-grants-2012_12 |
| ORD ID | ord-0646c067664e4abd8f11a6ac87460ef8 |
| 출처 메모 | uspto-grants-2012_12 |