反应详情

A suspension of 56 mg (1.47 mmol) of LiAlH4 in 2 ml of abs. THF is added to a suspension of 150 mg of 2-[(R)-(−)-2-carbamoyl-pyrrolidin-1-yl]-6-(3-chloro-phenyl-amino)-9-ethyl-9H-purine (cf. Example 45) in 10 ml of abs. THF and the mixture is stirred at 80° C. for 22 h. After further addition of 56 mg of LiAlH4, the mixture is allowed to react further for 18 h. 5 ml of WATER are then added dropwise, with ice/water cooling, and the reaction mixture is then poured onto 50 ml of ice/water. The mixture is extracted three times with ethyl acetate. The combined organic extracts are washed twice with water and once with saturated sodium chloride solution and dried over magnesium sulfate. After filtration, the filtrate is concentrated under reduced pressure. The resulting crude product (oil) is purified by means of column chromatography and digestion in diisopropyl ether. 2-[(R)-2-Aminomethyl-pyrrolidin-1-yl]-6-(3-chloro-phenyl-amino)-9-ethyl-9H-purine is obtained; m.p. 126–129° C.; FAB-MS: (M+H)+=372, HPLC: tret (grad20/2)=11.09 minutes.

1. customto react further for 18 h
2. extractionThe mixture is extracted three times with ethyl acetate
3. washThe combined organic extracts are washed twice with water and once with saturated sodium chloride solution
4. dry with materialdried over magnesium sulfate
5. filtrationAfter filtration
6. concentrationthe filtrate is concentrated under reduced pressure
7. customThe resulting crude product (oil) is purified by means of column chromatography and digestion in diisopropyl ether