反应详情

A mixture of 10.0 g of 4-p-nitrobenzamido-1,5-naphthalenedisulfonic acid disodium salt (prepared as in Example 3), 200 ml of water and 1.0 g of 10% palladium on charcoal is hydrogenated in a Parr shaker for 11/2 hours at room temperature with an initial pressure of 46 pounds of hydrogen. During this time a total of 4.5 pounds of hydrogen is absorbed. The mixture is heated to dissolve some precipitated product and is filtered hot to remove the catalyst. The filtrate is then evaporated to a small volume in vacuo at about 60° C. and a copious amount of absolute ethyl alcohol is added. The product is collected by filtration and is washed with absolute ethyl alcohol followed by ether. After air drying the material is oven dried at 120° C. overnight.

1. custom2 hours
2. customat room temperature
3. customDuring this time a total of 4.5 pounds of hydrogen is absorbed
4. temperatureThe mixture is heated
5. dissolutionto dissolve some precipitated product
6. filtrationis filtered hot
7. customto remove the catalyst
8. customThe filtrate is then evaporated to a small volume in vacuo at about 60° C.
9. additiona copious amount of absolute ethyl alcohol is added
10. filtrationThe product is collected by filtration
11. washis washed with absolute ethyl alcohol
12. customAfter air drying the material
13. customdried at 120° C. overnight