反应详情

1,1-dimethylethyl 7-(2-(methyloxy)-6-{[(4-methyl-2-pyridinyl)methyl]oxy}phenyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (2.57 g) was dissolved in dioxane (20 ml). Gaseous hydrogen chloride was passed through the reaction mixture for about 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 by silica column chromatography eluting with 0-8% methanol in DCM. The appropriate fractions were combined and concentrated in vacuo to yield a solid. This was triturated with diethyl ether to yield the title compound, 1.34 g (67%).

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 by silica column chromatography
11. washeluting with 0-8% methanol in DCM
12. concentrationconcentrated in vacuo
13. customto yield a solid
14. customThis was triturated with diethyl ether