Nitrogen → 2-(3-Chloropropyl)tetrahydrofuran

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.

1. temperaturethe mixture was refluxed for 3.5 h
2. concentrationconcentrated in vacuo
3. additionTo the residue was added water (30 mL)
4. extractionthe resulting mixture was extracted with DCM (30 mL×4)
5. washThe combined organic layers were washed with brine (40 mL×2)
6. dry with materialdried over anhydrous Na2SO4
7. concentrationconcentrated in vacuo

ORDレコード

ord-e292eb899bb543de8f436d55505c3500

出典データセット

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09434695B2