HCID 178473176, compound → HCID 178484300, compound

Participants

Reaction Steps

To 74 mg (0.11 mmole) of ethyl 2-[[(2R,3S)-3-(Boc-L-phenylalanyl-L-histidylamino)-4-cyclohexyl-2-hydroxy-1-butyl]thio]acetate was added 100 μl of N,N-dimethylethylenediamine. The mixture, which was stirred at room temperature in a stoppered flask, became homogeneous within a few minutes. After 18 hours, the mixture, which had gelled, was triturated thoroughly with hot ether. The resulting solid was collected on a filter and washed several times with ether, triturating thoroughly each time. This yielded 68 mg (86%) of white powder, mp 160°-164° (preliminary softening), virtually homogeneous by TLC (90:10:1 CHCl3 --MeOH-cond. NH4OH). Mass spectrum and 200 MHz NMR (DMSO d6) were in accord with the assigned structure.

Provenance & Evidence