1-(1-Ethoxyethyl)-1H-pyrazole synthesis

Yield:28791-95-9 93%

Reaction Conditions:

with trifluoroacetic acid in dichloromethane at 20 - 33;Large scale;

Steps:

General synthetic procedure for the synthesis of N-EtOEt protected pyrazole derivatives 1a-13a.

General procedure: To a solution of pyrazole 1-13 (1 equiv.) and trifluoroacetic acid (0.01 equiv.) in dichloromethane(for 1 mol of pyrazole - 1 L of dichloromethane were used) ethyl vinyl ether (1.27 equiv.) wasadded dropwise, keeping the temperature between 28-32 C (exothermic reaction) and left to stir atroom temperature for 12-78 hours. Dichloromethane was washed with saturated NaHCO3 solution(1 × 250 mL - for 1 L of dichloromethane) then with deionized H2O (1 × 250 mL). Organic layerwas dried with anhydrous Na2SO4, and evaporated under reduced pressure. Products were purifiedby distillation or recrystallization.

References:

Mazeikaite, Rita;Sudzius, Jurgis;Urbelis, Gintaras;Labanauskas, Linas [ARKIVOC,2014,vol. 2014,# 6,p. 54 - 71]