1,3-二氯-1,1,3,3,-四甲基二硅氧烷

反应条件: temp:-78.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Fifty (50) ml of n-butyl lithium (1.55 in hexane) were transferred via a syringe to a one-necked, round-bottomed flask, under nitrogen, equipped with a magnetic stirrer. Ten (10) grams of 3-Bromofuran in 10 ml of dry tetrahydrofuran (THF) were then added dropwise under nitrogen. Once this addition was complete, the resulting solution was stirred at -78 degrees C. for 1 hour. A pale yellow precipitate formed, and 6.5 g of 1,3-dichlorotetramethyl disiloxane in 10 ml dry THF were then added dropwise at -78 degrees C. under nitrogen. The precipitate slowly disappeared. The solution was then stirred for 4 hours at -78 degrees C. to a one-necked, round-bottomed flask, under nitrogen, equipped with a magnetic stirrer Once this addition A pale yellow precipitate formed The solution was then stirred for 4 hours at -78 degrees C

反应条件: temp:-78.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Fifty (50) ml of n-butyl lithium (1.55 in hexane) were transferred via a syringe to a one-necked, round-bottomed flask, under nitrogen, equipped with a magnetic stirrer. Ten (10) grams of 3-Bromofuran in 10 ml of dry tetrahydrofuran (THF) were then added dropwise under nitrogen. Once this addition was complete, the resulting solution was stirred at -78 degrees C. for 1 hour. A pale yellow precipitate formed, and 6.5 g of 1,3-dichlorotetramethyl disiloxane in 10 ml dry THF were then added dropwise at -78 degrees C. under nitrogen. The precipitate slowly disappeared. The solution was then stirred for 4 hours at -78 degrees C. to a one-necked, round-bottomed flask, under nitrogen, equipped with a magnetic stirrer Once this addition A pale yellow precipitate formed The solution was then stirred for 4 hours at -78 degrees C

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: There was added 2.6 moles of butyl lithium in hexane over a 15 minute period to a mixture of 50 grams of the 3-bromo-N,N-bis(trimethylsilyl)aniline in 400 ml. of anhydrous ether cooled to 0° C. under a nitrogen atmosphere. The resulting reaction mixture was allowed to stir for an additional 2 hours at 0° C. The mixture was then added to a mixture of 100 ml. of anhydrous ether and 16.06 grams of 1,3-dichloro-1,1,3,3-tetramethyldisiloxane at 0° C. After the solution was filtered and the solvents were removed under reduced pressure, there was obtained a 77% yield of 1,3-bis[N,N-bis(trimethylsilyl)-3-aminophenyl]-1,1,3,3-tetramethyldisiloxane in the form of a pale-yellow oil having a boiling point of about 169°-174° C. The resulting reaction mixture The mixture was then added to a mixture of 100 ml at 0° C After the solution was filtered the solvents were removed under reduced pressure

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: There was added 2.6 moles of butyl lithium in hexane over a 15 minute period to a mixture of 50 grams of the 3-bromo-N,N-bis(trimethylsilyl)aniline in 400 ml. of anhydrous ether cooled to 0° C. under a nitrogen atmosphere. The resulting reaction mixture was allowed to stir for an additional 2 hours at 0° C. The mixture was then added to a mixture of 100 ml. of anhydrous ether and 16.06 grams of 1,3-dichloro-1,1,3,3-tetramethyldisiloxane at 0° C. After the solution was filtered and the solvents were removed under reduced pressure, there was obtained a 77% yield of 1,3-bis[N,N-bis(trimethylsilyl)-3-aminophenyl]-1,1,3,3-tetramethyldisiloxane in the form of a pale-yellow oil having a boiling point of about 169°-174° C. The resulting reaction mixture The mixture was then added to a mixture of 100 ml at 0° C After the solution was filtered the solvents were removed under reduced pressure

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Diethylamine, 184 g. (2.50 mole) of 400 ml. of anhydrous ether were added to a one-liter multi-necked round bottom flask equipped with reflux condenser, pressure equalizing addition funnel, thermometer and stirrer, which was maintained under a positive pressure of argon. The solution was chilled with an ice water bath to 5°-10° C. during the dropwise addition of 100 g. (0.50 mole) of 1,3-dichloro-1,1,3,3,-tetramethyldisiloxane. After addition was completed the mixture was stirred overnight at room temperature (20°-25° C.). The mixture was then filtered and the filtrate was concentrated by rotary evaporation. The resulting residue was distilled at reduced pressure and yielded 81 g. (0.29 mole; 60% theoretical) of V (b.p. 75°-80° C., 2 mm. Hg.). equipped with reflux condenser addition funnel thermometer and stirrer, which was maintained under a positive pressure of argon The solution was chilled with an ice water bath to 5°-10° C. during the dropwise addition of 100 g After addition The mixture was then filtered the filtrate was concentrated by rotary evaporation The resulting residue was distilled at reduced pressure yielded 81 g

反应条件: temp:-78.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Fifty (50) ml of n-butyl lithium (1.55 in hexane) were transferred via a syringe to a one-necked, round-bottomed flask, under nitrogen, equipped with a magnetic stirrer. Ten (10) grams of 3-Bromofuran in 10 ml of dry tetrahydrofuran (THF) were then added dropwise under nitrogen. Once this addition was complete, the resulting solution was stirred at -78 degrees C. for 1 hour. A pale yellow precipitate formed, and 6.5 g of 1,3-dichlorotetramethyl disiloxane in 10 ml dry THF were then added dropwise at -78 degrees C. under nitrogen. The precipitate slowly disappeared. The solution was then stirred for 4 hours at -78 degrees C. to a one-necked, round-bottomed flask, under nitrogen, equipped with a magnetic stirrer Once this addition A pale yellow precipitate formed The solution was then stirred for 4 hours at -78 degrees C