反应详情

A mixture of the product from Example 31 Step 5 (0.17 g, 0.47 mmol), N-cyclohexylcarbodiimide,N′-methyl polystyrene resin (0.4 g, 0.65 mmol, 1.7 mmol/g), and 1-hydroxybenzotriazole hydrate (0.081 g, 0.6 mmol) were suspended in DMF (4 ml) and treated with triethylamine (0.084 ml, 0.6 mmol) and dimethylamino-acetic acid (0.048 g, 0.47 mmol). The reaction was stirred at room temperature for 16 hours and filtered on to a 10 g SCX cartridge (Varian Mega Bond Elute). The cartridge was then washed with methanol and then a 1:90.880 ammonia:methanol solution. The ammonia containing fractions were then reduced in vacuo and the residue purified by chromatography on silica gel eluting with a mixture of 0.880 ammonia/methanol/chloroform (0.5:4.5:95) to afford the title compound (0.097 g, 47%); MS (ES+) m/e 444 (M+H)+.

1. filtrationfiltered on to a 10 g SCX cartridge (Varian Mega Bond Elute)
2. washThe cartridge was then washed with methanol
3. customthe residue purified by chromatography on silica gel eluting with a mixture of 0.880 ammonia/methanol/chloroform (0.5:4.5:95)