反应详情

A mixture of 0.181 g of product from Example 17, 0.032 g of sodium bicarbonate, 2 ml of water, 11 ml of dioxane and 0.100 g of 10% palladium/carbon is reduced in a Parr apparatus at 42 psi of hydrogen for 3 hours. The reaction mixture is filtered through a pad of diatomaceous earth, washed with water and concentrated to 1/2 volume. The solution is extracted with ethyl acetate and the aqueous layer is freeze-dried. The product is purified using C18 reverse phase chromatography (95/5 water/ethyl alcohol) to give 0.095 g of the desired product as a yellow solid.

1. filtrationThe reaction mixture is filtered through a pad of diatomaceous earth
2. washwashed with water
3. concentrationconcentrated to 1/2 volume
4. extractionThe solution is extracted with ethyl acetate
5. customthe aqueous layer is freeze-dried
6. customThe product is purified