Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dibutylchloro(propyl)stannane → 5-(difluoromethoxy)-3-(tributylstannyl)-1H-indazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dibutylchloro(propyl)stannane | HCID 59914830 | — |
| 반응물 | 3-(5-(difluoromethoxy)-3-iodo-1H-indazol-1-yl)-N,N-dimethylpropan-1-amine | HCID 71279816 | — |
| 반응물 | HCID 178418918 | HCID 178418918 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 5-(difluoromethoxy)-3-(tributylstannyl)-1H-indazole | HCID 178448231 | — |
반응 단계
To a solution of 3-(5-(difluoromethoxy)-3-iodo-1H-indazol-1-yl)-N,N-dimethylpropan-1-amine (1.2 g, 2.78 mmol) in dry THF (25 mL) was added isopropylmagnesium chloride (1.5 mL, 2M in THF, 3 mmol) drop-wise at −16° C. under nitrogen atmosphere. The reaction was stirred for 30 minutes, then dibutylchloro (propyl)stannane (3.3 mL, 3.6 mmol) was added dropwise at −16° C. under nitrogen, then the reaction mixture was slowly warmed to room temperature and stirred for 2 hours. The reaction mixture was quenched with a solution of saturated NH4Cl (40 mL) and product extracted with EtOAc (3×30 mL), organics combined dried with sodium sulfate, filtered and concentrated. Crude oil used into the next step without further purification (1.1 g, crude).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08658646B2 |
| 출처 데이터셋 | uspto-grants-2014_02 |
| ORD ID | ord-564934e42e8c41d48052eebbcfd37fb0 |
| 출처 메모 | uspto-grants-2014_02 |