Yield:1443739-40-9 86%

Reaction Conditions:

with tris-(dibenzylideneacetone)dipalladium⁽⁰⁾;XPhos in tetrahydrofuran;diethyl ether at 60;

Steps:

1.A Step A: tert-butyl (2-aminopyrimidin-5-yl)acetate

To the solution of 2-amino-5-bromopyrimidne (3 g, 17.24 mmol) in 100 mL of THF were added Pd₂(dba)₃ (0.789 g, 0.862 mmol) and X-PHOS (0.882 g, 1.724 mmol), followed by 2-(tert- butyloxy)-2-oxoethylzinc chloride (86 mL, 0.5 M in ether). The reaction mixture was heated at 60 °C overnight. The reaction was diluted with saturated aqueous NH₄C1 (100 mL), and the aqueous layer extracted with EtOAc. The organic fractions were washed with brine, dried, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel eluting with 5-15% EtOAc:hexanes to afford 3.1 g (86%) of the title compound. Rf was 0.55 20% EtOAc in hexanes (blue spot on CAM stain). LC/MS (m/z): 210(M+H)+-

References:

WO2013/122821,2013,A1 Location in patent:Page/Page column 45