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Piperazine, 1-(hydroxyacetyl)-4-methyl- (9CI) synthesis

2synthesis methods
-

Yield:91406-27-8 12%

Reaction Conditions:

in 1,4-dioxane at 120;Sealed tube;

Steps:

Intermediate 66: 2-hydroxy-1-(4-methylpiperazin-1-yl)ethan-1-one

In a suitable flask, 1-methylpiperazine (2.9 mL, 26.15 mmol) was added to a mixture of 2-hydroxyacetic acid ethyl ester (3.09 mL, 32.66 mmol) in 1,4-Dioxane (5 mL).The flask was sealed and the reaction mixture was stirred overnight at 120 °C. The mixture was allowed to reach RT and concentrated under reduced pressure. The crude material was purified by flash chromatography on Biotage silica cartridge (from DCM to 4% MeOH) to afford Intermediate 66 (642 mg, 4.06 mmol, 12% yield) as a thick colorless oil. (0456) 1H NMR (400 MHz, Chloroform-d) δ ppm 4.16 (s, 2 H), 3.66 - 3.75 (m, 2 H), 3.25 - 3.34 (m, 2 H), 2.41 (q, J= 5.06 Hz, 4 H), 2.32 (s, 3 H).

References:

WO2022/13307,2022,A1 Location in patent:Page/Page column 110