Quenching method of active metal sodium or lithium
A technology of active metal and metal sodium, which is applied in the quenching of active metal sodium or lithium, and the field of active metal quenching, can solve the problems of increasing the difficulty of product separation and purification, and achieve the effect of increasing the operating safety factor and simple operation
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Embodiment 1
[0019] Example 1 The reaction equation is as follows:
[0020]
[0021] Under nitrogen protection, metal sodium (2.6 g, 0.11 mol) and 20 mL of toluene were heated to 100° C. until the metal sodium was completely dissolved, then began to stir rapidly and then continued to heat up to 105-110° C. Bis (tetrahydropyrrole) boron bromide (21.8g, 0.094mol) was dissolved in 6mL of toluene, and began to be added dropwise to the above-mentioned sodium metal toluene solution, and a weak reflux state was maintained during the dropwise addition. After hours, the system was dark blue, a small sample was taken for GC detection and the reaction was completed, and the internal standard yield of the calibration reaction solution was 79%. At this time, chlorocyclopentane (0.4mol) / toluene (15mL) solution was added dropwise, the addition was completed, and the reaction was stirred for 2 hours. At this time, the internal standard yield of the standard reaction solution was 78%, filtered, and the ...
Embodiment 2
[0023] Example 2 The reaction equation is as follows:
[0024]
[0025] Under nitrogen protection, sodium metal (22.3 g, 0.97 mol) and 78 mL of toluene were added to the reaction flask, and after the sodium metal melted, the temperature was raised to 105-110 ° C under rapid stirring, and bis(dimethylamino)boron bromide was added. (135.6g, 0.76mol) was dissolved in 55mL of toluene, and began to be added dropwise to the above-mentioned sodium metal toluene solution. During the dropwise addition, a weak reflux state was maintained. After the dropwise addition was completed, keep stirring for 3-5 hours. The system was dark blue. The GC detection reaction was completed, and the internal standard yield of the calibration reaction solution was 80%. At this time, bromo-n-hexane (0.6mol) / toluene (70mL) solution was added dropwise. After initiation, the dropping rate could be accelerated. The dropwise addition was completed in about 1 hour, and the reaction was stirred for 2 hours. A...
Embodiment 3
[0027] Example 3 The reaction equation is as follows:
[0028]
[0029] Under nitrogen protection, sodium metal (36g, 1.6mol) and 144mL of xylene were added to the reaction flask, and after the sodium metal melted, the temperature was raised to 135-145°C under rapid stirring, and bis(dimethylamino)boron chloride was added. (190g, 1.4mol) was dissolved in 95mL of xylene, and began to be added dropwise to the above-mentioned sodium metal toluene solution. During the dropwise addition, a weak reflux state was maintained. The GC detection reaction was completed, and the internal standard yield of the calibration reaction solution was 83%. At this time, isobutyl chloride (0.4mol) / toluene (110mL) solution was added dropwise, there was no obvious initiation process during the dropwise addition, the dropwise addition was completed, and the reaction was stirred for 2-3 hours. At this time, the internal standard yield of the calibration reaction solution was 83%. Filtration, the sol...
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