反应详情

温度

5 °C

Into a one liter flask equipped with a motorized stirrer is added 0.15 mole (25.17g, 98.47% pure) of 2,5-dimethyl-2,5-dihydroperoxyhexane and 0.15 mole (19.35g) of dichlorodimethylsilane in 400 ml of anhydrous ether. This mixture is cooled to about 5° C., and ammonia gas is introduced cautiously. Reaction temperature is maintained between 5° and 10° C. by use of an ice bath and by adjusting the rate of gas introduction. Ammonia addition is continued for 30 to 40 minutes until the exothermic reaction has stopped. The reaction mixture is then stirred at room temperature for an additional 3 hours. The salts are removed by filtration and the ether is removed by distillation. The crude yield of a colorless solid was 26.7 grams. To purify the crude product hexane is added and the mixture is filtered to remove a small amount of insoluble, unreacted 2,5-dimethyl-2,5-dihydroperoxyhexane. Evaporation of the hexane yields 21.9 grams (62.4%) of 3,3,6,6,9,9-hexamethyl-1,2,4,5-tetraoxa-3-silacyclononane having a melting point of 44.5°-48° C. The product is 95.5% pure based upon active oxygen (A.O.) analysis wherein theoretical A.O. is 13.67% and A.O. found is 13.05%. Analysis of the product supports the structure ##STR4## as follows: (1) I.R. spectrum indicates no terminal hydroperoxy (--OOH) groups; (2) the molecular weight corresponds to a cyclic structure; and (3) various chromatographic analyses verify a very non-polar species.

1. customInto a one liter flask equipped with a motorized stirrer
2. customReaction temperature
3. temperatureis maintained between 5° and 10° C. by use of an ice bath
4. customis continued for 30 to 40 minutes until the exothermic reaction
5. customThe salts are removed by filtration
6. customthe ether is removed by distillation
7. customTo purify the crude product hexane
8. additionis added
9. filtrationthe mixture is filtered
10. customto remove a small amount of insoluble, unreacted 2,5-dimethyl-2,5-dihydroperoxyhexane
11. customEvaporation of the hexane