反应详情

温度

120 °C

Mix under argon atmosphere 4-fluorobenzonitrile (1.21 g, 10 mmol), benzyl mercaptan (1.86 g, 15 mmol), and cesium carbonate (6.5 g, 20 mmol) in anhydrous NMP (20 mL). Degas the flask and fill with argon. Heat at 120° C. for 3 h. Cool to ambient temperature, dilute with EtOAc, filter and wash with 1N aqueous HCl. Separate the organic layer, dry over Na2SO4 and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (1:0 and 9:1) to obtain the desired intermediate (689 mg, 31%). GC-MS m/z: 225 (M+).

1. customDegas the flask
2. temperatureCool to ambient temperature
3. additiondilute with EtOAc
4. filtrationfilter
5. washwash with 1N aqueous HCl
6. customSeparate the organic layer
7. dry with materialdry over Na2SO4
8. concentrationconcentrate in vacuo
9. customPurify by chromatography on silica gel eluting with hexane/EtOAc (1:0 and 9:1)