反应详情

Tris(3,3-dimethylbutyl)tin chloride was prepared by the gradual addition of stannic chloride (13.0 g., 0.05 mole) dissolved in 50 c.c. pentane to a solution containing 19.5 g. (0.05 mole) of methyl tris(3,3-dimethylbutyl)tin dissovled in 50 c.c. pentane. The addition required 20 minutes and was performed under a nitrogen atmosphere. External cooling was applied as necessary to maintain the temperature of the reaction mixture below 27° C. Following completion of the addition the resulant mixture was heated at the boiling point for 0.5 hour, then allowed to cool to ambient temperature. A solution containing 2 c.c. of 12 normal aqueous hydrochloric acid and 100 c.c. water was added to the reaction mixture over a three minute period, followed by 50 c.c. of benzene. The organic liquid phase was separated, combined with 102 c.c. of an aqueous hydrochloric acid solution as previously described, after which the organic solvent was separated, dried using a portion of anhydrous magnesium sulfate and the organic solvents removed under reduced pressure. A 10 g. portion of the resultant white solid residue, obtained in 90% yield, was recrystallized from 100 c.c. of hexane and exhibited the following analysis, by weight:

1. dissolutiondissolved in 50 c.c
2. additionThe addition required 20 minutes
3. temperatureExternal cooling
4. temperatureto maintain the temperature of the reaction mixture below 27° C
5. additioncompletion of the addition the resulant mixture
6. temperaturewas heated at the boiling point for 0.5 hour
7. additionA solution containing 2 c.c
8. customThe organic liquid phase was separated
9. customafter which the organic solvent was separated
10. customdried
11. customthe organic solvents removed under reduced pressure
12. customportion of the resultant white solid residue, obtained in 90% yield
13. customwas recrystallized from 100 c.c