3,4-Difluoroanisole → 1-Fluoro-4-methoxy-2-methylsulfanylbenzene

温度

60 °C

1,2-Difluoro-4-methoxy-benzene (100 mg, 0.69 mmol) and sodium methanethiolate (148 mg, 2.08 mmol) were dissolved in N,N-dimethylformamide (2 mL) and the reaction mixture stirred at 60° C. for 18 hours. Additional sodium methanethiolate (99 mg, 139 mmol) was added and the reaction mixture heated to 100° C. for 18 hours. The reaction mixture was diluted with water and extracted with ether (x2). The ether extracts were washed with water (x2), dried over magnesium sulphate and concentrated in vacuo. The residue was taken up in pentane:ether 1:1 mixture (2 mL) and filtered through a plug of silica in a pipette, washing through with pentane:ether 1:1 mixture (5 mL). The solution was concentrated in vacuo to yield the title product as a colourless oil, 135 mg.

1. temperaturethe reaction mixture heated to 100° C. for 18 hours
2. extractionextracted with ether (x2)
3. washThe ether extracts were washed with water (x2)
4. dry with materialdried over magnesium sulphate
5. concentrationconcentrated in vacuo
6. filtrationfiltered through a plug of silica in a pipette
7. washwashing through with pentane:ether 1:1 mixture (5 mL)
8. concentrationThe solution was concentrated in vacuo

ORDレコード

ord-141050ea762b4c168e7b42b138ebb6c1

出典データセット

uspto-grants-2006_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07141586B2