2-(2-Oxocyclohexyl)-2-hydroxy-acetic acid methyl ester synthesis

Yield:352547-75-2 72%

Reaction Conditions:

with trifluoroacetic acid in toluene at 20; for 24 h;Aldol Condensation;

Steps:

9 Example 9: Synthesis of methyl 2-hydroxy-2-(2-oxocyclohexyl)acetate (III-2)

The reaction flask in 25mL 1.0g (5.7mmol) of methyl glyoxylate (II-2, mass fraction of a toluene solution of 50% II-2) and 5.6g (57mmol) cyclohexanone (I), was slowly added dropwise trifluoroacetic acid 32mg (0.28mmol), stirring at room temperature, 24h and concentrated under reduced pressure, the residue was purified by silica gel column chromatography (eluent: petroleum ether and ethyl acetate in a volume ratio of 2: 1) yielded 0.76g product methyl 2-hydroxy-2-(2-cyclohexyl)acetate (III-2), as a pale yellow oily liquid in a yield of 72.0%.

References:

CN104710305,2016,B Location in patent:Paragraph 0058; 0059; 0060; 0061