反应详情

To a stirred solution of 1,1-dimethylethyl 7-[2-({[4-(methyloxy)-2-pyridinyl]methyl}oxy)phenyl]-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (3.0 g) in dioxane (30 ml) was added hydrogen chloride gas for 2 h at 10-20° C. This was concentrated in vacuo. The residue was dissolved in water, washed with ethyl acetate and basified by adding aqueous sodium bicarbonate. This was extracted with 10% methanol in DCM. The organics were dried over sodium sulphate and concentrated in vacuo to yield the title compound, 2.14 g (91%).

1. concentrationThis was concentrated in vacuo
2. dissolutionThe residue was dissolved in water
3. washwashed with ethyl acetate
4. additionby adding aqueous sodium bicarbonate
5. extractionThis was extracted with 10% methanol in DCM
6. dry with materialThe organics were dried over sodium sulphate
7. concentrationconcentrated in vacuo