1-isopropylcyclohexyl Methacrylate

Chemical Properties

Colorless transparent liquid

Uses

1-Isopropylcyclohexyl methacrylate is used as photoresist monomer.

Preparation

The preparation of 1-isopropylcyclohexyl Methacrylate is as follows:23.5 g (3.4 mol) of lithium granules and 100 g of diethyl ether were weighed into a 2 L three-necked flask and protected by dry nitrogen.276.1 g (2.24 mol) of bromoisopropane, 100 g (1 mol) of cyclohexanone and 500 g of diethyl ether were weighed and mixed to form a preliminary liquid I, which was placed in a constant pressure dropping funnel at an internal temperature of 32 °C.5 mL of the preliminary solution I was added to the lithium particles. After the reaction was initiated, a large amount of heat was released, and the internal temperature was raised to 50 ° C, and the solution turned gray and white smoke appeared.When the internal temperature drops to 30 ° C, the preliminary liquid I is continuously added dropwise and stirring is started.Control the internal temperature 154.6 g (1.53 mol) of triethylamine and 10 g of phenothiazine were added.105.3 g (1.2 mol) of methyl methacrylate and 100 g of diethyl ether were weighed and mixed to form a preliminary liquid II, which was placed in a constant pressure dropping funnel.When the internal temperature of the reaction system was 35 ° C, the preliminary solution II was started to be added dropwise, and as the mixed solution was added dropwise, the reaction was slowly exothermic, and the internal temperature was controlled to be dropwise added at 50 ° C or lower.After 30 min, the reaction was stopped after incubation at 40 ° C for 2 h. After cooling to 25 ° C, the reaction solution was poured into 1 L of ice water and stirred for 40 min.The liquid phase was separated, and the aqueous phase was extracted with 150.0 g × 2 of diethyl ether. The organic phase was combined, washed with 50.0 g of 2 NaOH aqueous solution, washed with 200 g × 2 pure water, dried with 100.0 g of anhydrous sodium sulfate, filtered, and pumped with oil Distillation under reduced pressure gave 196.8 g of a colorless transparent liquid. The fluidity was good, and the nuclear magnetic spectrum confirmed the structure was correct. The purity of the GC was 99.72%, and the yield was 91.96%.