Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Silane, ((1-methoxy-2-methyl-1-propenyl)oxy)trimethyl- → HCID 59251137, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Silane, ((1-methoxy-2-methyl-1-propenyl)oxy)trimethyl- | HCID 552336 | — |
| 반응물 | 4-(1-(4-fluorophenyl)-1H-indazol-5-yl)tetrahydro-2H-pyran-4-ol | HCID 68706594 | — |
| 촉매 | Titanium Tetrachloride | HCID 24193 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | HCID 59251137 | HCID 59251137 | 99% |
반응 단계
To 4-(1-(4-fluorophenyl)-1H-indazol-5-yl)tetrahydro-2H-pyran-4-ol (125 mg, 0.40 mmol) in 5 mL of DCE was added TiCl4 (0.44 mmol; 0.44 mL of 1 M solution in DCM). A precipitate immediately formed. The reaction was concentrated in vacuo to approx 1 mL volume and treated with 1-methoxy-2-methyl-1-(trimethylsiloxy)propene (0.23 mL, 1.2 mmol) and the reaction became homogeneous and was complete. The reaction was quenched with NaHCO3, extracted 4× EtOAc, and combined organic layers were dried over MgSO4, filtered, and concentrated. The residue was purified by SiO2 chromatography using 25% EtOAc in hexanes to give methyl 2-(4-(1-(4-fluorophenyl)-1H-indazol-5-yl)tetrahydro-2H-pyran-4-yl)-2-methylpropanoate (155 mg, 99%). MS found: (M+H)+=397.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08198311B2 |
| 출처 데이터셋 | uspto-grants-2012_06 |
| ORD ID | ord-d4a5c1a8103045f8a4c58b27fb70af1d |
| 출처 메모 | uspto-grants-2012_06 |