反应详情

温度

60 °C

In a hydrogenator, 23 l of N,N-dimethylacetamide, 1.65 Kg (8.39 moles) of 5-chlorocarbonylphthalide (prepared for example as described in J. Chem. Soc., 1931, 867–871) and 200 g of 5% Pd/BaSO4 are charged Hydrogen is then charged at 3 bar thereinto and the mixture is heated at 60±3° C. for a total of 48 hours. The mixture is cooled and, after removal of the catalyst by filtration, the filtrate is concentrated under vacuum at 75° C. up to a solid residue. The product is dispersed with 8 l of deionized water and, at 5÷10° C. under stirring, the pH of the mixture is adjusted to 7.0÷7.5 by addition of 2.3 l of 10% ammonium hydroxide solution After a 30-minute stirring, the product is filtered, washed with deionized water and dried under vacuum at 50° C. to give 885 g (65%) of desired product having m.p.=163÷165° C. (in J. Chem Soc. 1925, page 2290 a m.p.=159÷160° C. is given).

1. additionis then charged at 3 bar
2. temperatureThe mixture is cooled
3. customafter removal of the catalyst
4. filtrationby filtration
5. concentrationthe filtrate is concentrated under vacuum at 75° C. up to a solid residue
6. additionThe product is dispersed with 8 l of deionized water and, at 5÷10° C.
7. additionthe pH of the mixture is adjusted to 7.0÷7.5 by addition of 2.3 l of 10% ammonium hydroxide solution After a 30-minute
8. stirringstirring
9. filtrationthe product is filtered
10. washwashed with deionized water
11. customdried under vacuum at 50° C.