Compounding technology of chloroethyl n-propyl ether
A technology for the synthesis of chloroethyl n-propyl ether, which is applied in the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., can solve the problems of low yield, cumbersome process, and large amount of waste water, and achieve purity and yield. High efficiency, clear and transparent appearance, and low water content
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Embodiment 1
[0029] Get 100g 2-n-propoxyethanol, 0.1g dodecyltrimethylammonium chloride and add in the reaction vessel with reflux condenser, add 120g thionyl chloride (content 99.0%, sulfuryl chloride content 0.1%) to constant Press the dropping funnel, start stirring, slowly add thionyl chloride dropwise to the reaction vessel, the reaction process releases sulfur dioxide and hydrogen chloride gas, control the rate of thionyl chloride addition to keep the temperature of the reaction solution at 30±5°C.
[0030] After the dropwise addition of thionyl chloride, turn on the heating, and gradually raise the temperature to 90°C according to the rate of reaction gas release, until no gas is released, and continue to keep warm for 2 hours to obtain the crude product; the crude product is directly purified by rectification to obtain 105.9 g of chloroethyl n-propyl ether, After testing, the chromatographic content of the product is 99.51%, the water content is 0.17%, and the yield reaches 89.97%. ...
Embodiment 2
[0032] Embodiment 1 rectification remaining bottom material 20g and 100g2-n-propoxyethanol, 0.01g benzyltriethylammonium chloride are added in the reaction vessel with reflux condenser, and embodiment 1 rectification produces fore distillation 12g and 123.4g thionyl chloride (content 98.0%, sulfuryl chloride content 0.3%) mixes, and starts to stir, and slowly adds dropwise this mixture in reaction vessel, and reaction process emits sulfur dioxide and hydrogen chloride gas, controls the rate of addition of thionyl chloride to make the reaction solution The temperature was maintained at 40±5°C.
[0033] After the dropwise addition, turn on the heating, and gradually raise the temperature to 95°C according to the reaction gas release rate until no gas is released, and continue to keep warm for 3 hours to obtain the crude product; the crude product is directly purified by rectification to obtain 116.01g of chloroethyl n-propyl ether. After testing, the product The chromatographic ...
Embodiment 3
[0035] Embodiment 2 Rectification remaining still bottom material 15g and 100g 2-n-propoxyethanol, 0.03g methoxymethyl triphenyl phosphine chloride are added in the reaction vessel with reflux condenser, and embodiment 2 rectification produces front Distill 6.5g and mix with 125.65g thionyl chloride (content 98.2%, sulfuryl chloride content 0.5%), start stirring, slowly add dropwise this mixture in reaction vessel, operating process is as embodiment 2.
[0036] After the dropwise addition, turn on the heating, and gradually raise the temperature to 100°C according to the reaction gas release rate, until no gas is released, and continue to keep warm for 4 hours to obtain the crude product; the crude product is directly purified by rectification to obtain 116.18g of chloroethyl n-propyl ether. After testing, the product The chromatographic content is 99.39%, the water content is 0.19%, and the yield reaches 98.70%.
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