反应详情

To a vigorously stirred mixture containing 970 g. (6.2 moles) of freshly distilled N1,N1 -diethyl-1,4 pentanediamine, 4 l. of 1,2-dichloroethane and 1 l. of water at 5°-10° C. there was simultaneously added dropwise a solution containing 5.95 moles of 4-chloro-2-nitrobenzoyl chloride in approximately 8 l. of 1,2-dichloroethane and a solution containing 410 g. (6.2 moles) of 85% potassium hydroxide in 1 l. of water. When the addition was complete the ice bath was removed and stirring was continued 0.5 hours at room temperature. The organic layer was separated, dried over anhydrous calcium sulfate and evaporated to dryness under vacuum. The residue was dissolved in 3 l. or 1,2-dichloroethane and the resulting solution was treated with decolorizing carbon and filtered. The filtrate was diluted to 6 l. with additional 1,2-dichloroethane to give a pale yellow solution of 4-choro-N-[4-(diethylamino)-1-methylbutyl]-2-nitrobenzamide which was divided into three equal portions which were used directly in the next step.

1. additionTo a vigorously stirred mixture containing 970 g
2. additionWhen the addition
3. customwas removed
4. customThe organic layer was separated
5. dry with materialdried over anhydrous calcium sulfate
6. customevaporated to dryness under vacuum
7. dissolutionThe residue was dissolved in 3 l
8. additionor 1,2-dichloroethane and the resulting solution was treated with decolorizing carbon
9. filtrationfiltered
10. additionThe filtrate was diluted to 6 l