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5,5-dimethyl-1,3-dioxane-2-propionaldehyde synthesis

4synthesis methods
-

Yield:58697-03-3 67%

Reaction Conditions:

with 2-Iodobenzoic acid in dichloromethane;dimethyl sulfoxide at 50; for 2 h;

Steps:

2

To a mixed solution of the alcohol S76-3 (2.1 g, 12.0 mmol, 1.0 equivalent) in a mixed solution of CH2Cl2 (40.0 mL) and DMSO (8.0 mL) was added 2-iodobenzoic acid (4.0 g, 14.4 mmol, 1.0 equivalent), and The reaction was heated to 50 ° C and held for 2 hours. After completion of the reaction (monitored by TLC), the reaction mixture was hydrolyzed with water, filtered on a pad of diatomaceous earth and extracted three times with CH2Cl2. The combined organic phases were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography (petroleum ether / ethyl acetate = 15/1) to obtain aldehyde S76-2 as a colorless liquid (1.4 g, 67% yield)

References:

CN110627610,2019,A Location in patent:Paragraph 0358-0360