反应详情

A 2 mL CH2Cl2 suspension of 0.05 g (0.11 mmol) 4-(cyclohexylamino)-8-[3-aminobenzyl]-1-(3-fluorophenyl)-1,3,8-triazaspiro[4.5]dec-3-en-2-one, 0.1 mL (0.11 mmol) acetyl chloride and excess K2CO3 was allowed to stir at rt overnight. The reaction was filtered and concentrated then the remaining oil was dissolved in 1 mL CH2Cl2 and purified on an Isco automated system affixed with a Biotage Flash 25(S) cartridge eluted at 20 mL/min with 0-5% MeOH in CH2Cl2 over 15 min and hold at 5% MeOH for 30 min. The product eluted second, pure by HPLC/MS and NMR.

1. filtrationThe reaction was filtered
2. concentrationconcentrated
3. dissolutionthe remaining oil was dissolved in 1 mL CH2Cl2
4. custompurified on an Isco automated system
5. washeluted at 20 mL/min with 0-5% MeOH in CH2Cl2 over 15 min
6. waithold at 5% MeOH for 30 min
7. washThe product eluted second, pure by HPLC/MS and NMR