1,2-Dichloroethane → HCID 86761386, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 7-{3-[4-(aminosulfonyl)piperazin-1-yl]propyl}-14-cyclohexyl-7,8-dihydro-6H-indolo[1,2-e][1,5]benzoxazocine-11-carboxylic acid (0.04 M) in DCM were added EDC (1.5 eq) and DMAP (3 eq). The mixture was stirred at 50° C. for 2 h before cooling to RT and evaporating all volatiles in vacuo. The residue was purified by RP-HPLC (Waters Sunfire column; MeCN/H2O/0.1% TFA gradient). Fractions containing the pure compound were combined and lyophilized to afford the product as a white powder (19%). 1H NMR (400 MHz, DMSO-d6+TFA, 335 K) 1.16-1.23 (m, 2H), 1.31-1.39 (m, 2H), 1.47-1.50 (m, 1H), 1.69-1.73 (m, 2H), 1.83-2.19 (m, 7H), 2.64-2.66 (m, 1H), 3.29-3.36 (m, 4H), 3.49-3.74 (m, 7H), 3.89-3.93 (m, 2H), 4.28-4.39 (m, 1H), 4.40-4.44 (m, 1H), 7.28-7.32 (m, 2H), 7.35-7.37 (m, 1H), 7.45-7.47 (m, 1H), 7.52-7.56 (m, 1H), 7.90-7.92 (m, 2H); (ES+) m/z 563 (M+H)+.

Provenance & Evidence