Chlorotrimethylsilane → HCID 131734593, compound

Temperature

25 °C

250 g (1.55 mol) of hexamethyldisilazane (((CH3)3Si)2NH) and 10 g (0.075 mol) of aluminum chloride (AlCl3) were put into 2000 mL of a flame-dried Schlenk flask under anhydrous and inert atmosphere while stirring, 499.80 g (3.87 mol) of dichloro dimethylsilane ((CH3)2SiCl2) was slowly added thereto while maintaining temperature of 25° C. and a temperature of the reaction solution was slowly raised to 40° C. The mixed reaction solution was stirred for 3 hours and the produced chlorotrimethylsilane ((CH3)3SiCl) and the excessively added dichloro dimethylsilane ((CH3)2SiCl2) were removed therefrom by simple distillation or distillation under reduced pressure. The recovered chloro dimethyl disilazane (((CH3)2SiCl)2NH)) solution was stirred and then 475.45 g (6.5 mol) of diethylamine ((CH3CH2)2NH) was slowly added thereto while maintaining temperature of −15° C. After the addition was completed, a temperature of the reaction solution was slowly raised to room temperature, and the reaction solution was stirred at room temperature for 6 hours. After the white solid obtained by filtration was removed to obtain a filtrate, solvent was removed from the filtrate under reduced pressure, and 319.90 g (1.16 mol) of diethylamino dimethyl disilazane ((CH3)2SiN(CH2CH3)2)2NH) was obtained by reduced pressure distillation with a yield of 75%.

1. temperaturea temperature of the reaction solution was slowly raised to 40° C
2. customThe mixed reaction solution
3. stirringwas stirred for 3 hours
4. customwere removed
5. distillationby simple distillation or distillation under reduced pressure
6. stirringThe recovered chloro dimethyl disilazane (((CH3)2SiCl)2NH)) solution was stirred
7. temperaturewhile maintaining temperature of −15° C
8. additionAfter the addition
9. temperaturea temperature of the reaction solution was slowly raised to room temperature
10. stirringthe reaction solution was stirred at room temperature for 6 hours
11. customAfter the white solid obtained by filtration
12. customwas removed
13. customto obtain a filtrate, solvent
14. customwas obtained by reduced pressure distillation with a yield of 75%

ORD record

ord-c3e76e172cb343afa797bbc02a534546

Source dataset

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09245740B2