ETHYL N-PHENYLFORMIMIDATE synthesis
- Product Name:ETHYL N-PHENYLFORMIMIDATE
- CAS Number:6780-49-0
- Molecular formula:C9H11NO
- Molecular Weight:149.19
Yield: 97%
Reaction Conditions:
with styrene-styrene sulfonic acid copolymer microspheres PS-HSSPS in water at 120; for 6 h;Temperature;
Steps:
3.1; 3.2; 3.3; 3.4; 3.5 Example 3
(1) In a round bottom flask equipped with a condenser and a thermometer, nitrogen was previously introduced for 15 min. Under nitrogen protection, the constant temperature water bathHeated to 60 ° C, 20 g of styrene, 50 mL of deionized water, 0.025 g of sodium hydroxide, 0.021 g of sodium hydrogencarbonate,After the system temperature reached 75 , add 1.4g potassium persulfate, the system was milky white liquid, and at this temperature for 4h,Polystyrene microspheres PS;(2) To the reaction solution at 75 ° C in step (1), 8 g of sodium styrene sulfonate was added and the reaction was continued for 3 hours. After filtration and drying,White solid, i.e., styrene-styrene sulfonate copolymer microspheres PS-NaSS PS;(3) The styrene-styrene sulfonate copolymer microspheres PS-NaSS PS obtained in the step (2) were mixed with 19.4 ml of hydrochloric acid(2 mol / L) was subjected to acidification treatment and then washed with water and dried at 40 ° C to obtain a styrene-styrene sulfonic acid copolymer microsphere PS-HSS PS with a particle size of 350 nm;(4) A 50 mL three-necked flask equipped with a thermometer and a water separator was charged with 0.089 mol of aniline, 0.15 mol of orthoformic acidTriethyl ester (having a mass of 22.27 g) and 0.125 g of PS-HSS PS prepared from step (3); heated to a constant temperature oil bath120 , stirring, with gas chromatograph every 1h monitoring reaction process, the reaction 6h to stop the reaction; the system cooled to room temperatureTo a dark yellow oily liquid, filtered to recover catalyst PS-HSS PS;(5) The filtrate obtained in step (4) was purified by distillation under reduced pressure to obtain N- (ethoxymethylene) aniline in a yield of97%.
References:
Hebei University of Science and Technology;Liu, Shaojie;Du, Huili;Cui, Xiaofei;Xing, Yubin;Zhao, Fengqing CN106117085, 2016, A Location in patent:Paragraph 0015; 0016; 0017; 0018; 0019; 0020
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