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ChemicalBook CAS DataBase List ISOPROPYL METHACRYLATE
4655-34-9

ISOPROPYL METHACRYLATE synthesis

5synthesis methods
-

Yield:-

Reaction Conditions:

with 2,2,6,6-Tetramethyl-1-piperidinyloxy free radical;4-methoxy-phenol at 108 - 118; under 52.5053 - 300.03 Torr;

Steps:

2 Example 2 (Preparation of the Catalyst by Ligand Exchange)
93.0 g of freshly distilled Al(Oi-Pr)3 were mixed with 70 mg of TEMPOL (4-hydroxy-2,2,6,6-tetramethylpiperidin-1-oxyl), 70 mg of HQME (hydroquinone monomethyl ether) and 300 g of MAMA and distilled within 3 h using a distillation column with introduction of air. The distillation started at a bottom temperature of 118° C. and a pressure of 400 mbar. The pressure was slowly reduced within three hours to 70 mbar, so that a steady but slow condensation was apparent at the condenser. The top temperature reached values of at most 108° C. here. Initially the isopropyl methacrylate produced and then the excess MAMA were distilled off via the distillation. The end of distillation was apparent from the rise of the bottom temperature from 115° C. to 133° C., reduced boiling and reduction of the top temperature. An orange, clear and viscous bottoms product (119 g) and a clear, colorless distillate (232 g) were obtained. The bottoms product was used without further purification as catalyst for methallyl methacrylate synthesis (with the assumption of 3.81 mmol of [Al] to 1 g of this bottoms product). GC analysis of the distillate gave 31.3% by weight of methallyl methacrylate and 68.7% by weight of isopropyl methacrylate, corresponding to the degree of ligand exchange of approx. 91%.

References:

EVONIK OPERATIONS GMBH;LYGIN, Alexander;KRILL, Steffen;GR?MPING, Matthias;TEPPERIS, Andreas US2020/148621, 2020, A1 Location in patent:Paragraph 0059

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