反应详情

To a solution of tert-butyl 4-(2-(2-chloropyridin-4-yl)-5-oxo-5H-[1,3,4]thiadiazolo[3,2-a]pyrimidin-7-yl)piperazine-1-carboxylate (160 mg, 0.36 mmol) in THF (5 ml) are added Boc-gly-NH2 (124 mg, 0.72 mmol), XantPhos (124 mg, 0.14 mmol), Pd(OAc)2 (24 mg, 0.07 mmol) and K2CO3 (197 mg, 1.44 mmol). The microwave tube is purged with nitrogen for 1 min then sealed. The mixture is microwaved at 90° C. for 2 h. After cooling to room temperature, EtOAc (30 ml) and water (30 ml) are added. The organic layer is separated, washed with brine and dried over sodium sulfate. After the removal of organic solvent in vacuo, the residue is purified through Biotage column chromatography (MeOH/DCM=1/100 to 5/20) to give the desired product (188 mg, 90%).

1. customThe microwave tube is purged with nitrogen for 1 min
2. customthen sealed
3. customThe mixture is microwaved at 90° C. for 2 h
4. additionEtOAc (30 ml) and water (30 ml) are added
5. customThe organic layer is separated
6. washwashed with brine
7. dry with materialdried over sodium sulfate
8. customAfter the removal of organic solvent in vacuo
9. customthe residue is purified through Biotage column chromatography (MeOH/DCM=1/100 to 5/20)