反应详情

1,1-dimethylethyl 7-(3-{[(4-methyl-2-pyridinyl)methyl]oxy}-2-pyridinyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (3.8 g) was dissolved in dioxane (20 ml). Gaseous hydrogen chloride was passed through the reaction mixture for 1.5 h. The reaction was monitored by TLC. On completion the solid formed was collected by filtration and washed with acetone. The solid was then dissolved in water and the mixture neutralised with aqueous sodium hydroxide (1M). The sticky solid formed was extracted with DCM. The organic phase was dried over sodium sulphate and concentrated in vacuo to give a solid. This was purified through silica, eluting the product with 0-12% methanol in DCM. The solid from this was triturated in diethyl ether to give the title compound, 2 g (69%) yield.

1. customOn completion the solid formed
2. filtrationwas collected by filtration
3. washwashed with acetone
4. dissolutionThe solid was then dissolved in water
5. customThe sticky solid formed
6. extractionwas extracted with DCM
7. dry with materialThe organic phase was dried over sodium sulphate
8. concentrationconcentrated in vacuo
9. customto give a solid
10. customThis was purified through silica
11. washeluting the product with 0-12% methanol in DCM
12. customThe solid from this was triturated in diethyl ether