Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

114340-52-2

Citric Acid tert-Butyl Ester synthesis

3synthesis methods
-

Yield:114340-52-2 86%

Reaction Conditions:

with sodium hydrogencarbonate in methanol;water at 0 - 20; for 5.25 h;

Steps:

A2 Molecule 4: Product Obtained by Saponification of Molecule 3

Molecule 4: Product Obtained by Saponification of Molecule 3 (0333) To a solution of molecule 3 (3.35 g, 12.13 mmol) in methanol (120 mL) at 0° C., a 2N aqueous solution of soda (18.2 mL), cooled beforehand to 0° C., is added. The medium is stirred at 0° C. for 15 min, then at ambient temperature for 5 h. After evaporation of the organic phase under a vacuum, the medium is diluted with water (50 mL), and the aqueous phase is washed with ethyl acetate (100 mL), then acidified with a 10% aqueous solution of HCl and extracted with ethyl acetate (2×150 mL). The organic phase is washed with water (100 mL), a saturated aqueous solution of NaCl (150 mL), then dried over Na2SO4, filtered and evaporated under a vacuum, to yield a white solid. The aqueous phase is extracted again with ethyl acetate (2×150 mL), dried over Na2SO4, filtered and evaporated under a vacuum to yield a second portion of the desired product. (0334) Yield: 15.6 g (86%) (0335) 1H NMR (CD3OD, ppm): 1.46 (9H); 2.71 (2H); 2.86 (2H). (0336) LC/MS (ESI): 247.1; (calculated ([M-H]-): 247.3).

References:

US2017/136097,2017,A1 Location in patent:Paragraph 0333; 0334; 0335; 0336