반응 #91563

반응 방정식

1,1-dimethylethyl 7-(5-acetyl-2-{[(4-methyl-2-pyridinyl)methyl]oxy}phenyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate

hydrogen chloride

→

title compound

1-[4-{[(4-methyl-2-pyridinyl)methyl]oxy}-3-(2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl)phenyl]ethanone

용매

dioxane

반응 조건

후처리

1. 1
   기타On completion the solid formed
2. 2
   여과was collected by filtration
3. 3
   세척washed with acetone
4. 4
   workup.DISSOLUTIONThe solid was then dissolved in water
5. 5
   기타Solid was obtained which
6. 6
   여과was collected by filtration
7. 7
   기타This was triturated with diethyl ether

실험 절차

1,1-dimethylethyl 7-(5-acetyl-2-{[(4-methyl-2-pyridinyl)methyl]oxy}phenyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (3.0 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). Solid was obtained which was collected by filtration. This was triturated with diethyl ether to yield the title compound, 2.1 g (88%).

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