反应详情

In analogy to the method described in example B1, 3.0 g (7.8 mmol) of (3-benzyloxy-4-methoxy-benzyl)(5-chloro-2,6-dimethylpyrimidin-4-yl)amine (from example A4) are reacted with 30 ml of 12.5N hydrochloric acid in 30 ml of ethanol. Extraction with ethyl acetate at a pH of 8 gives, after concentration, a solid residue which is chromatographed on silica gel (mobile phase: toluene/dioxane=5:1). Crystallization from toluene/methanol gives 1.86 g (72%) of the title compound as a beige crystallizate. m.p.: 165-168° C.

1. extractionExtraction with ethyl acetate at a pH of 8
2. customgives
3. concentrationafter concentration
4. customa solid residue which is chromatographed on silica gel (mobile phase: toluene/dioxane=5:1)
5. customCrystallization from toluene/methanol