反应详情

温度

-20 °C

n-Butyllithium (26.02 ml, 1.55M in hexane) was added dropwise over thirty minutes to a stirred solution of trimethylsilylacetylene (5.18 ml) in dry tetrahydrofuran (25 ml), whilst maintaining the temperature below -65° C. After twenty minutes, diethylchlorophosphite (4.71 ml) was added dropwise over twenty minutes, then stirring continued for a further ninety minutes at -65° C. The stirred mixture was allowed to warm to -20° C., quenched by dropwise addition of saturated ammonium chloride solution (10 ml), then allowed to reach room temperature, diluted with water (10 ml) and extracted with chloroform (4×25 ml). The extracts were dried over magnesium sulphate and evaporated under reduced pressure to give diethyl trimethylsilylethynylphosphonite as a brown oil (7.34 g, 83% pure by GC).

1. temperaturewhilst maintaining the temperature below -65° C
2. waitAfter twenty minutes
3. waitcontinued for a further ninety minutes at -65° C
4. customquenched by dropwise addition of saturated ammonium chloride solution (10 ml)
5. customto reach room temperature
6. additiondiluted with water (10 ml)
7. extractionextracted with chloroform (4×25 ml)
8. dry with materialThe extracts were dried over magnesium sulphate
9. customevaporated under reduced pressure