反应详情

As described in example 1(a), the reaction is carried out with 130.7 g (0.5 mol) of 4-chloro-N-(4-methoxyphenyl)-benzamide, 24.5 g (1 mol) sodium hydride, 700 cc. of dimethylformamide and 118.5 g (0.5 mol) of 8-bromocaprylic acid methyl ester. Reaction time and reaction temperature: 5 hours at 80° C., thereafter 12 hours at 100° C. The reaction mixtures are further processed as described in example 1(a). The crude product is dissolved in 300 cc. of ether. After standing for a prolonged period, the unreacted 4-chloro-N-(4-methoxyphenyl)-benzamide separates by crystallisation and is filtered off. The solvent is partly distilled off and the resulting oily crude product (181 g) is separated. 125 g are used in the next step without further purification, the remainder (56 g) is purified chromatographically on silicic acid using chloroform as eluant.

1. customReaction time and reaction temperature
2. custom5 hours
3. customat 80° C.
4. custom12 hours
5. customat 100° C
6. customThe reaction mixtures
7. waitAfter standing for a prolonged period
8. customthe unreacted 4-chloro-N-(4-methoxyphenyl)-benzamide separates by crystallisation
9. filtrationis filtered off
10. distillationThe solvent is partly distilled off
11. customthe resulting oily crude product (181 g) is separated
12. custom125 g are used in the next step without further purification
13. customthe remainder (56 g) is purified chromatographically on silicic acid