Potassium thiocyanate → 2-(4-Bipenylyl)ethylthiocyanate

Bromine (1.5 ml) was added dropwise to an acetonitrile (60 ml) solution of triphenylphosphine (5 g). After stirring for 5 minutes, an acetonitrile solution (30 ml) of 2-(4-biphenylyl)ethanol (5 g) was added to the reaction mixture. The reaction mixture was stirred at room temperature for one hour and concentrated. Diethyl ether was added to the residue. The supernatant was collected, then dried and concentrated. The residue was purified by silica gel column chromatography (eluent: IPE) to obtain 2-(4-bipenylyl)ethylbromide(6 g). 2-(4-Bipenylyl)ethyl bromide (6 g) was dissolved in methanol (100 ml), which was stirred at 70° C. for 48 hours together with potassium thiocyanate (4.0 g). The reaction mixture was concentrated, and the residue was extracted with ethyl acetate. The organic layer was washed with water, then dried and concentrated. The residue was recrystallized from ethyl acetate-hexane to obtain the entitled compound (4.1 g).

1. concentrationThe reaction mixture was concentrated
2. extractionthe residue was extracted with ethyl acetate
3. washThe organic layer was washed with water
4. customdried
5. concentrationconcentrated
6. customThe residue was recrystallized from ethyl acetate-hexane

ORDレコード

ord-51729724afe44607b0ba2feef59384a5

出典データセット

uspto-grants-2001_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06329389B1