反应详情

A mixture of 25.0 g of 4-(m-nitrobenzamido)-1,5-naphthalenedisulfonic acid disodium salt (prepared as in Example 5), 200 ml of water and 2.0 g of 10% palladium on charcoal is hydrogenated in a Parr shaker for 4 hours and 20 minutes at room temperature with an initial pressure of 42 pounds of hydrogen. During this time a total of 11.0 pounds of hydrogen is absorbed. The mixture is heated to dissolve some precipitated product and is filtered through diatomaceous earth to remove the catalyst. The filtrate is then evaporated to a small volume in vacuo at 55°-60° C. until crystal formation. The material is then diluted with absolute ethyl alcohol and is triturated. The crystals are then collected by filtration and the product is washed first with two 100 ml portions of absolute ethyl alcohol followed by two 100 ml portions of ether. The product of the example is then oven dried overnight at 120° C.

1. customDuring this time a total of 11.0 pounds of hydrogen is absorbed
2. temperatureThe mixture is heated
3. dissolutionto dissolve some precipitated product
4. filtrationis filtered through diatomaceous earth
5. customto remove the catalyst
6. customThe filtrate is then evaporated to a small volume in vacuo at 55°-60° C. until crystal formation
7. additionThe material is then diluted with absolute ethyl alcohol
8. customis triturated
9. filtrationThe crystals are then collected by filtration
10. washthe product is washed first with two 100 ml portions of absolute ethyl alcohol
11. customoven dried overnight at 120° C.