15%MeOH/DCM: 2ml/11ml + triethyl amine: 5 drops (0.4 ml); Almost no starting material was seen. However, the Rf value was too big. Rf(product) = 4.7/5.1 = 0.92; Rf(1,4-Bis(3-aminopropyl) piperazine) = 0.5/4.4 = 0.113
5%MeOH/DCM: 0.5ml/9.5ml + triethyl amine: 0.3 ml; Two spots were accidentally left for the product next to each other; Rf prod = 1.2 / 3.4 = 0.35; Rf epoxide = >0.95; Rf amine = 0.07;
Reaction was left to run for 1 more day. TLC: 5%MeOH/DCM: 0.5ml/9.5ml + triethyl amine: 0.3 ml; TLC showed presence of product and epoxide and no signs of NH2, indicating that the reaction has gone to completion. RF product = 0.38; RF epoxide = 9.25; RF NH2 = 0.09
After 2 days, the product was taken out of the freezeer, it became yellowish solidified liquid. The weight of the unpurified compound was measured: 4.224 g.