反应详情

To a stirred solution of 3,5-Diamino-6-chloro-pyrazine-2-carboxylic acid ((S)-2-amino-pentyl)-amide hydrochloride (Example 4) (0.2 g, 0.73 mmol) in DMF (3 mL) is added triethylamine (0.22 mL, 1.54 mmol) followed by {[(Z)-tert-Butoxycarbonylimino]-pyrazol-1-yl-methyl}-[3-(4-methoxy-phenyl)-propyl]-carbamic acid tert-butyl ester (Intermediate E) and the resulting deep yellow solution is stirred at RT for 3 days. The reaction mixture is diluted with water (50 mL) and extracted with EtOAc (100 mL). The organic phase is washed with water (50 ml), dried (MgSO4), and the solvent removed in vacuo to afford a yellow oil. Chromatography (SiO2, EtOAc:iso-hexane, gradient 0-100%) affords (S,E)-tert-butyl 1-(3,5-diamino-6-chloropyrazin-2-yl)-7-(3-(4-methoxyphenyl)propyl)-10,10-dimethyl-1,8-dioxo-4-propyl-9-oxa-2,5,7-triazaundecan-6-ylidenecarbamate as a colourless oil. [M+H]+ 663.

1. extractionextracted with EtOAc (100 mL)
2. washThe organic phase is washed with water (50 ml)
3. dry with materialdried (MgSO4)
4. customthe solvent removed in vacuo
5. customto afford a yellow oil