2-PHENYL-5-METHYL-1,3-DIOXANE-5-CARBOXYLIC ACID synthesis

Yield:207850-04-2 82.3%

Reaction Conditions:

with toluene-4-sulfonic acid in toluene; for 8 h;Reflux;

Steps:

1.1 EXAMPLE 1

[0028] 1) To a 100 mL single-mouth bottle 0.80 g (5 9 mmol) of 2,2-dimethylol propionic acid, 0.63 g (5.9 mmol) of benzaldehyde, 0.1 g of p-toluenesulfonic acid, and 40 mL of toluene were added to form a solution. The solution was then heated and refluxed for 8 h. Thereafter, the solution was cooled to room temperature and a product precipitated in a decompression condition. 30 mL of saturated sodium carbonate aqueous solution was added to the solution to from a mixture. After being stirred for 20 min, the mixture was transferred to a separating funnel, and was extracted by using 30 mL×3 of ether whereby separating an aqueous phase from an organic phase. A 2 N sulfuric acid was then added to the aqueous phase to neutralize the pH value thereof. Finally, the aqueous phase was filtrated and dried to a constant weight to yield intermediate II-1, the formula of which is as follows. 1.09 g of the intermediate II-1 was obtained, and the yield thereof was 82.3%.

References:

US2013/296572,2013,A1 Location in patent:Paragraph 0028