(NE)-N-pentan-2-ylidenehydroxylamine synthesis
- Product Name:(NE)-N-pentan-2-ylidenehydroxylamine
- CAS Number:623-40-5
- Molecular formula:C5H11NO
- Molecular Weight:101.15
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Yield: 95.4%
Reaction Conditions:
with ammonium hydroxide;dihydrogen peroxide at 70; for 6 h;Molecular sieve;Temperature;
Steps:
1-15 Example 1:
A method for synthesizing 2-pentanone oxime by ammoxidation of 2-pentanone, using 2-pentanone, ammonia water and hydrogen peroxide as raw materials, the operation steps are as follows:
Weigh 50g of ammonia water with a mass concentration of 13.6% (the molar amount of NH3 in ammonia water is 0.4mol) and transfer it to the first constant pressure dropping funnel.Weigh 34g of hydrogen peroxide with a mass concentration of 30% (the molar amount of H2O2 molecules in hydrogen peroxide is 0.3mol) and transfer it to the second constant pressure dropping funnel for standby.In a 250mL three-necked flask, add 17.22g (0.2mol) of 2-pentanone as raw material,Then add 1.7g of F-Ti-MOR catalyst (the mass content of Ti in the catalyst is 3%),Warm to 70 , stir vigorously,At the same time, ammonia and hydrogen peroxide are slowly added dropwise through the first constant pressure dropping funnel and the second constant pressure dropping funnel,Ammonia and hydrogen peroxide were added dropwise in about 1 hour, and then the sealed reaction was continued at 70 ° C for 5 hours.After the reaction is completed, the catalyst is recovered by filtration, and then the organic layer is separated into liquids.After drying over anhydrous sodium sulfate and distillation under reduced pressure, 19.5 g (0.19 mol) of 2-pentanone oxime product was obtained.The yield was 95.4% and the purity was 99%.
References:
Zhejiang University of Technology;Li Xiaoqing;Xu Dawang;Xu Xiangsheng CN110981750, 2020, A Location in patent:Paragraph 0016-0031
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