1,2-Dichloroethane → HCID 23382104, compound

Participants

Reaction Steps

12.3 ml (88 mmol) of triethylamine are added to a solution of 3.3 g (17.6 mmol) of N-methoxycarbonyl-(L)-tert-leucine, 6.7 g (35.2 mmol) of EDC and 4.8 g (35.2 mmol) of HOBT in 90 ml of DMF (degassed under vacuum) and the whole is stirred at RT for 20 min. After that, 4 g (8.8 mmol) of 1-[p-(pyrrolidin-1-yl)phenyl]-4(S)-hydroxy-2-(tert-butyloxycarbonyl)amino-5(S)-amino-6-phenyl-2-azahexane (Example 8d), dissolved in 20 ml of DMF, are added and the mixture is stirred at RT for 16 h. The reaction mixture is concentrated by evaporation and the residue is taken up in ethyl acetate/water. The organic phase is separated off and subsequently washed consecutively with water, 5% sodium bicarbonate solution (twice), water, dilute brine and brine, with the title compound thereby being obtained. The solvent is removed and the residue is recrystallized from ether in an ice bath, with the title compound thereby being obtained.

Provenance & Evidence