Dichloromethane → 3,3-Diethoxypropanoic acid

To a solution of 25 g of ethyl 3,3-diethoxypropionate (131 mmol) in 79 mL of methanol there are added 13.1 mL of aqueous 35% sodium hydroxide solution (452 mmol). The reaction mixture is stirred at ambient temperature for 3 hours. The reaction mixture is then concentrated to remove the methanol. After dissolving the undissolved material by adding water, aqueous 5N HCl solution is added to obtain a pH of 5. Dichloromethane is added and then the organic phase is washed with brine. After drying over MgSO4 and concentrating to dryness, the title product is obtained in the form of an oil which is used in the next Step without being otherwise purified.

1. concentrationThe reaction mixture is then concentrated
2. customto remove the methanol
3. dissolutionAfter dissolving the undissolved material
4. additionby adding water, aqueous 5N HCl solution
5. additionis added
6. customto obtain a pH of 5
7. washthe organic phase is washed with brine
8. dry with materialAfter drying over MgSO4
9. concentrationconcentrating to dryness

ORD record

ord-91ecc06887ee464a9ddcbdd53316a71b

Source dataset

uspto-grants-2015_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09108983B2