O-TERT-BUTYLCYCLOHEXYL ACETATE synthesis
- Product Name:O-TERT-BUTYLCYCLOHEXYL ACETATE
- CAS Number:88-41-5
- Molecular formula:C12H22O2
- Molecular Weight:198.3
Yield:88-41-5 110.9 g
Reaction Conditions:
with toluene-4-sulfonic acid at 100 - 110;
Steps:
f; g; h
f) Open the e) step rotary evaporator to raise the temperature. Under normal pressure, the kettle temperature is 60 to 90°C, petroleum ether is recovered, and the collected petroleum ether is concentrated and reused.The vacuum pump was turned on, and the o-tert-butyl cyclohexanol was collected under a pressure of 1000 to 1333 Pa at a pot temperature of 95 to 100° C. The collected o-tert-butyl cyclohexanol was transferred to a four-necked flask.The bottom liquid is p-tert-butyl cyclohexanol, which can be used for the production of the appetite ester after collection.g) Adding 120 g of acetic anhydride and 3.5 g of p-toluenesulfonic acid to the four-necked flask, turning on the stirrer, turning on the cold and heat exchange integrated machine for heating, and controlling the reaction temperature at 100 to 110° C. for a reaction time of 3 to 5 hours.The reaction solution was transferred to a rotary evaporator and acetic acid was recovered under atmospheric pressure. The bottom liquid was transferred to a beaker.h) 25 g of 5% sodium hydroxide solution was metered in the beaker, the stirrer was turned on, and the collected oil layer was subjected to alkaline washing. After stirring for 0.5 hour, the mixture was allowed to stand for 0.5 hours and the lye layer was concentrated in the waste liquid collection drum.The oil layer was further added with 60 g of clear water for washing. After stirring for 0.5 hours, the mixture was allowed to stand for 0.5 hours. The water layer was concentrated in the waste liquid collection tank and washed twice.The oil layer was transferred to a rotary evaporator, and a rotary evaporator was turned on to raise the temperature. A vacuum pump was turned on and o-tert-butyl cyclohexyl acetate was collected to obtain 110.9 g of o-tert-butylcyclohexyl acetate.
References:
Anhui Huaye Flavors Hefei Co., Ltd.;Wang Tianyi;Wang Yang;Zhang Zheng;He Yunfei;Xu Jilong;Li Fangjie;Li Liping CN107879932, 2018, A Location in patent:Paragraph 0015; 0016; 0017
