反应详情

温度

0 °C

1.85 g (9.42 mmol) 2 phenyl-1,3-dithian was placed in a dry 50-ml three-necked flask under argon and dissolved in 28 ml anhydrous THF. 3.99 ml 2.36 M BuLi solution in hexane was added dropwise at 0° C. and the reaction solution stirred for 2 h at 0° C. 0.83 mg (3.93 mmol) diethyldichlorogermanium dissolved in 8 ml anhydrous THF was added slowly dropwise at 0° C. to the reaction mixture and then stirred for an additional 2 h at 0° C. To complete the reaction a further solution of 2-phenyl-2-lithium-1,3-dithian (2.36 mmol) was prepared as described above and added dropwise at 0° C. to the reaction solution, which was then stirred for 18 h at 6° C. The reaction was quenched by the addition of 20 ml water and the raw product extracted with diethyl ether (3×30 ml). The combined organic phases were dried with Na2SO4 and the solvent drawn off at the rotary evaporator. The residue was separated off by column chromatography (petroleum ether: ethyl acetate=20:1). 1.42 g (70% of the theoretical value) diethylbis(2-phenyl-1,3-dithian-2-yl)germanium was obtained as colorless solid. DC (petroleum ether: ethyl acetate=20:1): Rf=0.51

1. additionwas added slowly dropwise at 0° C. to the reaction mixture
2. stirringstirred for an additional 2 h at 0° C
3. customthe reaction a further solution of 2-phenyl-2-lithium-1,3-dithian (2.36 mmol)
4. customwas prepared
5. additionadded dropwise at 0° C. to the reaction solution, which
6. stirringwas then stirred for 18 h at 6° C
7. customThe reaction was quenched by the addition of 20 ml water
8. extractionthe raw product extracted with diethyl ether (3×30 ml)
9. dry with materialThe combined organic phases were dried with Na2SO4
10. customthe solvent drawn off at the rotary evaporator
11. customThe residue was separated off by column chromatography (petroleum ether: ethyl acetate=20:1)