ChemicalBook CAS DataBase List 3,5,5-trimethylcyclohex-3-en-1-one

3,5,5-trimethylcyclohex-3-en-1-one synthesis

7synthesis methods

Product Name:3,5,5-trimethylcyclohex-3-en-1-one
CAS Number:471-01-2
Molecular formula:C9H14O
Molecular Weight:138.21

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Yield: 98.3%

Reaction Conditions:

at 206; under 750.075 Torr; for 48 h;Catalytic behavior;Inert atmosphere;Pressure;Temperature;

Steps:

1
The 10gLa (NO 3) 3 was dissolved in 200ml of deionized water dubbed salt solution in La (NO 3) 3: NiFe 2 O 4 (Zibo Technology Co., Ltd.) = 15: 1 (mass ratio), the amount of salt added to NiFe 2 O 4 Solution, stir, dipping 8 hours. After filtration 60 ° C drying 8h; muffle furnace and then baked at 600 ° C Burn 3h, to obtain magnetic nanometer solid base catalyst La 2 O 3 / NiFe 2 O 4.At the bottom of the rectification column 1m previously added 10g La 2 O 3 / NiFe 2 O 4 and 200gα- isophorone. Nitrogen Reaction system was replaced three times at 206 ° C, 0.1MPa conditions, the plate number of 20, a reflux ratio of 3, stable Total reflux 1h, the tower, the tower began to adopt a kettle, bottom feed α- start isophorone flow rate of 100g / h feed Line continuous reactive distillation. After 48h, selective gas chromatography analysis determined β- isophorone is 99.7%; Overhead was collected to give the crude product β- isophorone (β- isophorone content of 65wt%). further Carried out in the two refined 0.2kPa, 0.2kPa pressure, plate number 25, a reflux ratio of R = 1.6, a temperature of 103 ° C, Feed tray position 13, produced fluids and bottom feed ratio D / F = 0.4975, and the overhead distillate feed ratio W / F = 0.5025, availability of> 99.5% purity β- isophorone, β- isophorone overall yield of 98.3%.

References:

Wanhua Chemical Group Co.,Ltd;Dong, Yanfeng;Zhang, Tao;He, Guangwen;Guo, Jinzi;Cui, Qian;Wang, Peng;Cong, Xin;Zhao, Jing;Chen, HaiBo;Li, Yuan;Hua, Weiqi CN104761443, 2016, B Location in patent:Paragraph 0035-0037

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10276-21-8 Synthesis