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Acetamide, N-[2-hydroxy-1-(hydroxymethyl)ethyl]- synthesis

6synthesis methods
-

Yield:2655-79-0 85.9%

Reaction Conditions:

in methanol;ethyl acetate;

Steps:

6.6A [0385] STEP 6A: Synthesis of compound 4_2

[0386] Compound 4_1 (20.0 g, 219 mmol, 1.00 eq) was added to a vessel containing Py (120 mL) at 25 °C. Ac2O (24.6 g, 241 mmol, 22.6 mL, 1.10 eq) was introduced dropwise in the reaction at 0 °C and then stirred for 1 h at 25 °C. TLC (Dichloromethane: Methanol = 5:1, Rf = 0.35) showed the reaction completed. Concentrated the reaction mixture to dryness and dissolved in ethyl acetate (60 mL). A precipitate was formed after stirring for 10 min at 5 °C. The precipitate was filtered and dried under vacuum. Compound 4_2 (25.1 g, 188 mmol, 85.9% yield) was obtained as white solid and it was used in the next reaction without further purification.

References:

WO2020/247782,2020,A1 Location in patent:Paragraph 0384-0386