N,N'-Dimethylethylenediamine → HCID 59485614, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 1-Boc-3-oxopiperazine (1.0 eq.), 3-bromothiophene (1.5 eq.), K3PO4(2.0 eq.), CuI (0.4 eq.) and N,N′-dimethylethylendiamine (0.8 eq.) in 1,4-dioxane (0.5M) was put in a sealed vial and stirred at 110° C. for 18 hr. Reaction mixture was diluted with EtOAc and filtered through a pad of SolcaFloc® 200 FCC. After removal of the solvent, the crude product was purified by flash column chromatography on silica gel using 10-40% EtOAc/Petroleum ether as eluent to afford the desired product H1 as pink solid (80% yield). 1H NMR (400 MHz, CDCl3, 300K) δ 7.32-7.28 (3H, m), 4.25 (2H, s), 3.82-3.75 (4H, m), 1.49 (9H, s). MS (ES) C13H18N2O3S requires: 282, found: 283 (M+H)+.

Provenance & Evidence