반응식
[O:1]1[CH2:5][CH2:4][CH2:3][CH:2]1[CH2:6][CH2:7][CH2:8]O.[Cl:10]S(Cl)=O.N#N>>[Cl:10][CH2:8][CH2:7][CH2:6][CH:2]1[CH2:3][CH2:4][CH2:5][O:1]1참가 물질
4
실험 절차
To 3-(tetrahydrofuran-2-yl)propan-1-ol (3.90 g, 30.0 mmol) was added dichlorosulfoxide (15 mL) dropwise under N2 and the mixture was refluxed for 3.5 h. It was then cooled to rt and concentrated in vacuo. To the residue was added water (30 mL) and the resulting mixture was extracted with DCM (30 mL×4). The combined organic layers were washed with brine (40 mL×2), dried over anhydrous Na2SO4 and concentrated in vacuo to give the title compound as yellow liquid, which was used for next step without further purification.
후처리
- temperaturethe mixture was refluxed for 3.5 h
- concentrationconcentrated in vacuo
- additionTo the residue was added water (30 mL)
- extractionthe resulting mixture was extracted with DCM (30 mL×4)
- washThe combined organic layers were washed with brine (40 mL×2)
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-e292eb899bb543de8f436d55505c3500
- 출처 데이터셋
- uspto-grants-2016_09
- 특허 번호
- US09434695B2
연결된 노트
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