1-Bromo-4-(trans-4-propylcyclohexyl)benzene synthesis

Yield:86579-53-5 82%

Reaction Conditions:

with sodium hypochlorite;bromine at 20; for 2 h;

Steps:

2 Specific Example 2: Preparation of propylcyclohexyl bromobenzene (see Figure 4 for specific reaction equation)

202g of ethylcyclohexylbenzene,37.2g of sodium hypochlorite was put into a 500ml three-necked flask, and the temperature was lowered to 20 ° C with stirring, 80g of bromine was added to a constant pressure dropping funnel, and the temperature was kept and slowly added dropwise.After about 2h, the addition is completed and the heat is kept for 2h.Sampling test is qualified (propyl cyclohexylbenzene <2%, if it is unqualified, continue to keep warm, sampling and testing every 1h);Add H2O to the bottle, stir and let stand for layers, repeat until PH = 7;Add 2 times the mass of absolute ethanol to the organic phase in the bottle, stir to warm to boiling, keep boiling and reflux for 1h, cool to 0 ° C, filter with suction, and repeat again.Put the filter cake into the flask and raise the temperature until the white solid starts to melt. Turn on the stirring until it is completely melted. The temperature is raised and evacuated. After drying, 231.3g of white solid product is obtained (HPLC GC = 99.6%)Theoretical output: 282g propylcyclohexyl bromobenzeneYield = 231.3 / 282 * 100% = 82.0%

References:

CN111072446,2020,A Location in patent:Paragraph 0032-0038; 0048