反应详情

To the resulting oily residue of p-(8-cyclohexyloctyl)aminobenzoyl chloride hydrochloride is added, in one portion, the previously prepared mixture of sodium benzenesulfonamide in dimethylacetamide. The mixture is stirred for 30 minutes, without cooling, and is then filtered through a bed of diatomaceous earth. The filtrate is poured into 2 l. of water, and 250 ml. of saturated sodium chloride solution is added to coagulate the precipitate. The mixture is filtered and the product is washed with water and partially air dried. The product is dissolved in methylene chloride, the mixture is filtered through diatomaceous earth, and brine is added to break the emulsion. The layers are separated, the organic phase is dried over anhydrous sodium sulfate and filtered through a bed of 300 g. of hydrous magnesium silicate. The product is eluted with an additional 3 l. of methylene chloride. The first approx. 1 l. of filtrate is set aside and the remainder is evaporated to dryness. The residue is crystallized three times from toluene to yield the product.

1. temperaturewithout cooling
2. filtrationis then filtered through a bed of diatomaceous earth
3. additionThe filtrate is poured into 2 l
4. additionof saturated sodium chloride solution is added
5. filtrationThe mixture is filtered
6. washthe product is washed with water and partially air
7. customdried
8. dissolutionThe product is dissolved in methylene chloride
9. filtrationthe mixture is filtered through diatomaceous earth, and brine
10. additionis added
11. customThe layers are separated
12. dry with materialthe organic phase is dried over anhydrous sodium sulfate
13. filtrationfiltered through a bed of 300 g
14. washThe product is eluted with an additional 3 l
15. customthe remainder is evaporated to dryness
16. customThe residue is crystallized three times from toluene
17. customto yield the product