Triacetoxyperiodinane → Methyl 2-(7-chloro-2-(3-chlorophenyl)-5-methylpyrazolo[1,5-a]pyrimidin-6-yl)-2-oxoacetate

To a mixture of methyl 2-(7-chloro-2-(3-chlorophenyl)-5-methylpyrazolo[1,5-a]pyrimidin-6-yl)-2-hydroxyacetate (5 g, 13.65 mmol) in CH2Cl2 (20 mL) was added Dess-MartinPeriodinane (6.37 g, 15.02 mmol) and the reaction mixture was stirred at room temp for 1 h. The reaction mixture was diluted with ethyl acetate (100 mL). The organic layer was washed with saturated NaHCO3 solution (100 mL) and dried (Na2SO4). The solvent was evaporated and the residue was purified by a quick silica gel chromatography to afford (3.8 g, 76%) of the title compound. 1H NMR (500 MHz, CHLOROFORM-d) δ 8.10-7.98 (m, 1H), 7.89 (td, J=4.4, 1.5 Hz, 1H), 7.51-7.36 (m, 2H), 7.00 (s, 1H), 4.00 (s, 3H), 2.62 (s, 3H).

1. washThe organic layer was washed with saturated NaHCO3 solution (100 mL)
2. dry with materialdried (Na2SO4)
3. customThe solvent was evaporated
4. customthe residue was purified by a quick silica gel chromatography

ORDレコード

ord-380cca842d714eb6827abbaae20a531a

出典データセット

uspto-grants-2014_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08633200B2