反应详情

A solution of 7-chloro-1,3,4,5-tetrahydro3-hydroxy-3-(methoxycarbonyl)-4-(4-methoxyphenyl)-2H-1-benzazepin-2-one (0.5 g, 1.33 mmole) and lithium iodide (0.178 g, 1.33 mmole) in dry pyridine (20 ml) was refluxed under argon until complete conversion to product by TLC. The reaction was cooled to room temperature and concentrated in vacuo. The residue was dissolved in chloroform and extracted twice with 1N hydrochloric acid, once with saturated sodium chloride, and dried over magnesium sulfate. The solvent was removed in vacuo and the residue was triturated with ether to yield 0.22 g of the cis product.

1. concentrationconcentrated in vacuo
2. dissolutionThe residue was dissolved in chloroform
3. extractionextracted twice with 1N hydrochloric acid, once with saturated sodium chloride
4. dry with materialdried over magnesium sulfate
5. customThe solvent was removed in vacuo
6. customthe residue was triturated with ether
7. customto yield 0.22 g of the cis product