反应详情

温度

-55 °C

A solution of butyllithium (0.6M) (74 ml) in n-hexane are mixed with 116 ml of diethyl ether and cooled to -55° C. Thereupon, a solution of 40.0 g of 5-bromo-2,2-diphenyl-1,3-benzodioxol in 170 ml of diethyl ether is added dropwise. The reaction mixture is stirred for 1 hour, whereby the temperature rises to -15° C. Subsequently, the mixture is cooled to -50° C. and dry sulphur dioxide gas is introduced for 45 minutes. The excess sulphur dioxide gas is removed by passing dry argon through the mixture for 1 hour. The reaction mixture is left to come to room temperature. There thereby results a white precipitate, which is filtered off and dried. There are obtained 22.2 g of 2,2-diphenyl-1,3-benzodioxol-5-sulphinic acid lithium salt as white crystals of m.p.>300° C. (dec.).

1. customrises to -15° C
2. temperatureSubsequently, the mixture is cooled to -50° C.
3. customThe excess sulphur dioxide gas is removed
4. customfor 1 hour
5. waitThe reaction mixture is left
6. customto come to room temperature
7. customThere thereby results a white precipitate, which
8. filtrationis filtered off
9. customdried