Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → N-(5'-Bromospiro[cyclobutane-1,2'-indene]-3'(1'H)-ylidene)-2-methylpropane-2-sulfinamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Tert-Butanesulfinamide | HCID 3382465 | — |
| 반응물 | 6'-Bromospiro[cyclobutane-1,2'-inden]-1'(3'H)-one | HCID 67979616 | — |
| 촉매 | Titanium tetraethoxide | HCID 76524 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | HCID 178479889 | HCID 178479889 | — |
| 생성물 | N-(5'-Bromospiro[cyclobutane-1,2'-indene]-3'(1'H)-ylidene)-2-methylpropane-2-sulfinamide | HCID 67979440 | 135.3% |
반응 단계
6′-Bromospiro[cyclobutane-1,2′-inden]-1′(3′H)-one (Intermediate 38, 1.1 g, 4.38 mmol), 2-methylpropane-2-sulfinamide (0.96 g, 7.88 mmol), and titanium ethoxide (1.805 mL, 8.76 mmol) were dissolved in methyl THF (20 mL), and heated to reflux overnight. The reaction was allowed to cool to r.t., then it was diluted with EtOAc (150 mL). Water (22 mL) was added dropwise over 10 min under vigorous stirring and then the mixture was left standing without stirring for 1.5 h. The solids were filtered off and the organics were evaporated to give a crude product which was purified by flash chromatography (eluent: heptane/ethylacetate 8:1) to afford the title compound (2.1 g, 77% yield), used as such in the next step: MS (ES+) m/z 354 [M+H]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09248129B2 |
| 출처 데이터셋 | uspto-grants-2016_02 |
| ORD ID | ord-946b4d24b76842dcb3297b92e0afdeaf |
| 출처 메모 | uspto-grants-2016_02 |