反应详情

温度

92.5 °C

A mixture of methyl (2E)-3-(5-chloro-2-pyrazinyl)acrylate (10.00 g), tert-butyl (3R)-3-amino-1-pyrrolidinecarboxylate (14.01 g) and potassium phosphate (21.30 g) in DMA (25 mL) was stirred at 90-95° C. for 6 hours under nitrogen atmosphere. After addition of water, the reaction mixture was extracted with AcOEt. Water was added to the organic layer and the mixture was adjusted to pH 8 with 1N HCl aq., washed with water, dried over magnesium sulfate and concentrated under reduced pressure to give a residue. The residue was purified by silica gel (chromatorex NH) (hexane-AcOEt 60:40 v/v) to give tert-butyl (3R)-3-({5-[(1E)-3-methoxy-3-oxo-1-propen-1-yl]-2-pyrazinyl}amino)-1-pyrrolidinecarboxylate as a solid (10.64 g).

1. extractionthe reaction mixture was extracted with AcOEt
2. additionWater was added to the organic layer
3. washwashed with water
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customto give a residue
7. customThe residue was purified by silica gel (chromatorex NH) (hexane-AcOEt 60:40 v/v)