反应详情

Intermediate 1 (1.2 g, 4.76 mmol), Intermediate 50 (0.79 g, 5.2 mmol) and diisopropylethylamine (4 ml, 24 mmol) in MeCN (8 ml) was heated at 70° C. for 24 hours. The solvent was removed in vacuo and the residue partitioned between DCM and water. The organic phase was concentrated in vacuo and the residue chromatographed on silica (50 g) eluting with cyclohexane:ethyl acetate (2:1 followed by 1:1 then 1:2). Appropriate fractions were combined and evaporated to give Intermediate 51 as a brown oil (1.21 g). LCMS showed MH+=334; TRET=2.61 min.

1. customThe solvent was removed in vacuo
2. customthe residue partitioned between DCM and water
3. concentrationThe organic phase was concentrated in vacuo
4. customthe residue chromatographed on silica (50 g)
5. washeluting with cyclohexane:ethyl acetate (2:1
6. customevaporated