반응 #1364754

반응 방정식

caustic soda

6-t-butyl-3-(butylaminomethyl)-2,4-dimethylphenol

1,3-benzenedisulfonyl chloride

→

crude product

수율 100.1%

N,N'-Dibutyl-N,N'-Bis(4-t-butyl-3-hydroxy-2,6-dimethylbenzyl)-m-Benzenedisulfonamide

수율 100.1%

용매

acetone

water

반응 조건

후처리

1. 1
   온도while maintaining the temperature at 25°-30° C.
2. 2
   온도by cooling
3. 3
   온도while maintaining the temperature at 25°-30° C.
4. 4
   온도by cooling
5. 5
   기타to come to room temperature
6. 6
   기타the upper layer is separated
7. 7
   workup.ADDITIONslowly treated with ice water (100 mls)
8. 8
   workup.WAITupon standing for 2.5 hours
9. 9
   여과The solid is then recovered by filtration

실험 절차

To a stirred solution of 6-t-butyl-3-(butylaminomethyl)-2,4-dimethylphenol (5.26 grams; 0.02 mole) in acetone (40 mls) is slowly added 1,3-benzenedisulfonyl chloride (2.75 grams; 0.01 mole) while maintaining the temperature at 25°-30° C. by cooling. To this mixture is slowly added a solution of 50% caustic soda (1.6 grams; 0.02 mole) in water (22 mls) while maintaining the temperature at 25°-30° C. by cooling. The mixture is allowed to come to room temperature and stirred for 15 hours. The mixture is then allowed to settle, and the upper layer is separated and slowly treated with ice water (100 mls). The resulting oil which separates solidifies upon standing for 2.5 hours. The solid is then recovered by filtration to obtain the crude product (7.3 grams; 100% of theoretical). Recrystallization of the crude product from glacial acetic acid affords the pure product (2.5 grams; m.p. 143°-144.5° C.).

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