3-Bromo-1-propanol → HCID 9989971, compound

Temperature

80 °C

4-Fluorobenzenethiol (788 mg, 6.15 mmol) and 3-bromopropanol (0.535 ml, 6.16 mmol) was dissolved in tetrahydrofuran (20 ml). The solution was added with 1N aqueous solution of sodium hydroxide (6.2 ml, 6.2 mmol) and heated at 80° C. for 3 hours with stirring. The reaction mixture was diluted with a mixed solvent of ethyl acetate-hexane and washed with diluted aqueous solution of sodium hydroxide, water, and then with saturated brine, and dried over magnesium sulfate. Insoluble solids were moved by filtration and the filtrate was concentrated under reduced pressure. The resulting oil was purified by silica gel column chromatography (ethyl acetate-hexane) to obtain the title compound as colorless oil (592 mg, yield: 52%).

1. washwashed with diluted aqueous solution of sodium hydroxide, water
2. dry with materialwith saturated brine, and dried over magnesium sulfate
3. filtrationInsoluble solids were moved by filtration
4. concentrationthe filtrate was concentrated under reduced pressure
5. customThe resulting oil was purified by silica gel column chromatography (ethyl acetate-hexane)

ORD record

ord-c7c61dcf0f8248219914bf9031baffba

Source dataset

uspto-grants-2007_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07166617B2