反应详情

A mixture of EXAMPLE 56B (0.60 g, 2.60 mmol) and trans-cyclohexane-1,4-diamine (1.04 g, 9.08 mmol) in ethanol (10 mL) was heated at in a Biotage Initiator microwave reactor at 170° C. for 80 minutes. After concentration, the residue was treated with 20% brine and extracted twice with ethyl acetate. The combined organic layers were concentrated and purified on a 110 g silica column (KP-NH from Biotage) eluting with ethyl acetate/methanol (97:3 to 90:10) to give the title compound.

1. concentrationAfter concentration
2. additionthe residue was treated with 20% brine
3. extractionextracted twice with ethyl acetate
4. concentrationThe combined organic layers were concentrated
5. custompurified on a 110 g silica column (KP-NH from Biotage)
6. washeluting with ethyl acetate/methanol (97:3 to 90:10)