Ethanone, 1-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)- synthesis

7synthesis methods

Product Name:Ethanone, 1-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)-
CAS Number:54030-34-1
Molecular formula:C12H14O3
Molecular Weight:206.24

39235-58-0 Synthesis

1-[4-HYDROXY-3-(HYDROXYMETHYL)PHENYL]ETHANONE

39235-58-0
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Ethanone, 1-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)-

54030-34-1
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Yield:54030-34-1 93%

Reaction Conditions:

Stage #1: 4-hydroxy-3-hydroxymethylacetophenone;2,2-dimethoxy-propanewith toluene-4-sulfonic acid in dichloromethane;
Stage #2: 2,2-dimethoxy-propane in dichloromethane at 20;

Steps:

1.1; 1.2 1. Synthesis of 1-(2,2-dimethyl-4H-benzo[d][1,3]dioxan-6-yl)ethanone

(1) Add 33.23g of 4-hydroxy-3-hydroxymethylacetophenone and 3.23g of catalytic amount of p-toluenesulfonic acid (catalyst) to a 250mL three-necked flask, then add 100mL of dichloromethane (organic solvent) and stir Dissolve to light yellow reaction solution.(2) Add a mixed solution of 2,2-dimethoxypropane 41.49g and 60mL dichloromethane (organic solvent) to the reaction solution slowly at room temperature, continue stirring until the reaction is complete, add saturated carbonic acid to the reaction solution Adjust the reaction system to weakly alkaline with sodium hydrogen solution, let stand for layering, and separate the organic layer. The organic phase is washed with saturated aqueous sodium chloride solution and water, dried with anhydrous sodium sulfate, filtered to remove sodium sulfate, concentrated, and vacuum After drying, 38.34 g of light yellow oily liquid was obtained with a yield of 93%.

References:

CN110963929,2020,A Location in patent:Paragraph 0035-0040