反应详情

To a stirred solution of 1,1-dimethylethyl 7-(3-{[(4-ethyl-2-pyridinyl)methyl]oxy}-6-methyl-2-pyridinyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate, (4.3 g) in dioxane (30 ml) was passed through HCl (gas) for 30 min at 20° C. After completion of reaction by TLC, the solvent was removed in vacuo. The solid obtained was washed with acetone and dissolved in water. This was neutralised with sodium bicarbonate, extracted with DCM and concentrated in vacuo to give a crude product. This was purified through silica using 6% methanol in DCM. Appropriate fractions were combined and concentrated in vacuo to give a product. This was triturated in diethyl ether to yield the title compound, 1.5 g.

1. customAfter completion of reaction by TLC
2. customthe solvent was removed in vacuo
3. customThe solid obtained
4. washwas washed with acetone
5. dissolutiondissolved in water
6. extractionextracted with DCM
7. concentrationconcentrated in vacuo
8. customto give a crude product
9. customThis was purified through silica using 6% methanol in DCM
10. concentrationconcentrated in vacuo
11. customto give a product
12. customThis was triturated in diethyl ether