反应详情

A solution of 7-chloro-1,3,4,5-tetrahydro-3-hydroxy-3-(methoxycarbonyl)-4-(4-methoxyphenyl)-2H-1-benzazepin-2-one (16.4 g, 43.7 mmole) and lithium iodide (23.7 g, 174.6 mmole) in 290 ml of pyridine containing 1% water was refluxed under argon until complete conversion to product by TLC (ca. 1.5 hours). The reaction was cooled to room temperature and concentrated in vacuo. The residue was dissolved in ethyl acetate and extracted with 1N hydrochloric acid, saturated sodium bicarbonate and saturated sodium chloride. The solution was dried over magnesium sulfate and concentrated. The residue was recrystallized from ethyl acetate to afford 6.8 g of pure cis product.

1. concentrationconcentrated in vacuo
2. dissolutionThe residue was dissolved in ethyl acetate
3. extractionextracted with 1N hydrochloric acid, saturated sodium bicarbonate and saturated sodium chloride
4. dry with materialThe solution was dried over magnesium sulfate
5. concentrationconcentrated
6. customThe residue was recrystallized from ethyl acetate
7. customto afford 6.8 g of pure cis product