反应详情

温度

60 °C

{9-[(2R,3R,4S,5R)-3,4-Dihydroxy-5-(methoxymethyl)tetrahydro-2-furanyl]-6-[(2,2-diphenylethyl)amino]-9H-purin-2-yl}methyl methanesulfonate (preparation 25) (75 mg, 0.13 mmol) was added to a solution of 2,6dimethyl-3-pyridinylamine (22 mg, 0.17 mmol) and triethylamine (0.036 ml, 0.26 mmol) in ethyl acetate (3 ml) and N,N-dimethylformamide (1 ml) in the reaction vessel of a Argonaut Quest 210 machine. The reaction mixture was agitated and heated to 60° C. for 12 hr. More 2,6-dimethyl-3-pyridinylamine (22 mg, 0.17 mmol) and triethylamine (0.036 ml, 0.26 mmol) were added and heating and agitation continued for a further 24 hr. The reaction mixture was then washed with water and the organic phase separated and dried with anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give a residue which was purified by reverse phase HPLC using firstly a Lana C8 (2) column and then a Magellan C18 column eluting with 5 mM ammonium acetate in water:2 mM ammonium acetate in acetonitrile (90:10) decreasing in polarity to 5 mM ammonium acetate in water:2 mM ammonium acetate in acetonitrile (10:90) as eluant. This gave the title compound (9 mg) as a gum. MS: 596 (MH+).

1. temperatureheating
2. washThe reaction mixture was then washed with water
3. customthe organic phase separated
4. dry with materialdried with anhydrous magnesium sulfate
5. customThe solvent was removed under reduced pressure
6. customto give a residue which
7. customwas purified by reverse phase
8. washa Magellan C18 column eluting with 5 mM ammonium acetate in water