反応 #2355562
ord-47e7616990cc49269b70b82bdb7e0e36
反応方程式
反応物
試薬
反応条件
後処理
- 1温度heating
- 2洗浄The reaction mixture was then washed with water
- 3その他the organic phase separated
- 4乾燥dried with anhydrous magnesium sulfate
- 5その他The solvent was removed under reduced pressure
- 6その他to give a residue which
- 7その他was purified by reverse phase
- 8洗浄a Magellan C18 column eluting with 5 mM ammonium acetate in water
実験手順
{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+).