反应详情

温度

70 °C

A 2 N solution of lithium hydroxide was heated to 70° C. Methyl 4-(4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)-L-prolinate (Example 52, 0.081 g, 0.20 mM) in acetonitrile (1.1 ml) and water (0.4 ml) was added to the solution and stirred at 70° C. for ten minutes then ambient temperature for twenty minutes. 1 N Hydrogen chloride was added and a minor impurity was extracted using EtOAc. The aqueous layer was lyophilized to give an orange solid that was purified by HPLC eluting CH3CN/H2O (0.1% TFA). Relevant fractions were collected, concentrated and lyophilized to give the desired product as a light orange solid (0.039 g).

1. waitambient temperature for twenty minutes
2. extractiona minor impurity was extracted
3. customto give an orange solid
4. customthat was purified by HPLC
5. washeluting CH3CN/H2O (0.1% TFA)
6. customRelevant fractions were collected
7. concentrationconcentrated