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1,2-bis(o-tolyloxy)ethane synthesis

5synthesis methods
-

Yield:53223-37-3 89.49%

Reaction Conditions:

with sodium hydroxide in water at 70 - 75; for 8.3 h;Inert atmosphere;Reflux;Green chemistry;

Steps:

2 Example 2:

A process for preparing a thermal sensitizer characterized by adding 89.1 g (0.9 mol) of dichloroethane and 200 g (1.85 mol) of o-cresol and 35 ml of water to a kettle,While stirring under nitrogen gas, 100 g of a 49% (by weight) aqueous sodium hydroxide solution was added dropwise over 20 minutes,After the addition was complete, the mixture was refluxed under heating for 3 hours and then 72 g of 49% aqueous sodium hydroxide solution was added dropwise over 2 hours. Then, the solution was transferred to a separator and the aqueous layer was discharged. The oil layer was transferred back to the reaction vessel to continue condensation at 70 to 75C The reaction for 3 hours, diverting the amount of water 95ml, then add 175ml water heated to 100 stirring, standing,203.9 g of a crude organic layer of 1,2-bis (3-methylphenoxy) ethane (HPLC: 96.8%, yield 93.62%) was obtained by layering. The crude product was purified by distillation to obtain 194.9 g of 1,2-bis 2-methylphenoxy) ethane (HPLC detection: purity 99.5%, yield 89.49%).

References:

CN103772159,2017,B Location in patent:Paragraph 0015; 0016; 0019