Synthetic method of di(trimethylsilyl)phosphite
A technology of trimethylsilyl and phosphite, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as long reaction time, low purity, and high energy consumption problem, to achieve the effect of reducing energy consumption and cost, and lowering the reaction temperature
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[0020] Example 1
[0021] The humidity of the operating room is controlled at 46%-56%, and the temperature is about 25°C.
[0022] First, the phosphorous acid is subjected to dewatering operation, the phosphorous acid and toluene are placed in the container, and the oil bath is heated to reflux, and the water is separated for 4 hours. The water is removed, and the toluene is concentrated by rotary evaporation (water pump, vacuum degree 0.095MPa, temperature 60℃). To 2h to constant weight, the phosphorous acid after water removal is obtained.
[0023] Weigh 29.2g (0.356mol) of dewatered phosphorous acid and 90mL of formamide (102g) into a 500mL four-necked flask, pour in nitrogen, control the flow rate of nitrogen to 2ml / min, stir vigorously for about 20min, phosphorous acid After dissolving, a colorless transparent liquid is obtained, and the nitrogen gas is continuously introduced and exhausted for 30 minutes.
[0024] Add 140mL (120g, 1.1mol) trimethylchlorosilane (slightly brown) ...
Example Embodiment
[0028] Example 2
[0029] The humidity of the operating room is controlled at 46%-56%, and the temperature is about 25°C.
[0030] First, the phosphorous acid is subjected to dewatering operation, the phosphorous acid and toluene are placed in the container, and the oil bath is heated to reflux, and the water is separated for 4 hours. The water is removed, and the toluene is concentrated by rotary evaporation (water pump, vacuum degree 0.095MPa, temperature 60℃). To 2h to constant weight, the phosphorous acid after water removal is obtained.
[0031] Weigh 29.2g (0.356mol) of dewatered phosphorous acid and 90mL of formamide (102g) into a 500mL four-necked flask, pour in nitrogen, control the flow rate of nitrogen to 2ml / min, stir vigorously for about 20min, phosphorous acid After dissolving, a colorless transparent liquid is obtained, and the nitrogen gas is continuously introduced and exhausted for 30 minutes.
[0032] Add 140mL (120g, 1.1mol) of trimethylchlorosilane (slightly brow...
Example Embodiment
[0037] Example 3
[0038] The humidity of the operating room is controlled at 35%-45%, and the temperature is about 25°C.
[0039] First, the phosphorous acid is subjected to dewatering operation, the phosphorous acid and toluene are placed in the container, and the oil bath is heated to reflux, and the water is separated for 4 hours. The water is removed, and the toluene is concentrated by rotary evaporation (water pump, vacuum degree 0.095MPa, temperature 60℃) To 2h to constant weight, the phosphorous acid after water removal is obtained.
[0040] Weigh 29.2g (0.356mol) of dewatered phosphorous acid and 90mL of formamide (102g) into a 500mL four-neck flask, pour in nitrogen, control the flow rate of nitrogen to 5ml / min, and stir vigorously for about 15min. After dissolving, a colorless transparent liquid is obtained, and nitrogen gas is continuously introduced and exhausted for 20 minutes.
[0041] Add 180mL (152g, 1.4mol) of trimethylchlorosilane (slightly brown) to this colorless...
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