반응 #1364755

반응 방정식

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

1,3-benzenedisulfonyl chloride

sodium hydroxide

→

desired product

수율 32.7%

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

수율 32.7%

용매

water

acetone

water

반응 조건

후처리

1. 1
   온도maintaining the temperature at 30°-35° C
2. 2
   기타After separating the oily layer
3. 3
   workup.ADDITIONtreating the same with ice water
4. 4
   기타crystallization
5. 5
   여과the solid is filtered
6. 6
   기타to obtain the crude product (15.5 grams; 92% of theoretical)
7. 7
   기타Recrystallization of the crude product
8. 8
   workup.ADDITIONfrom a mixture of benzene and cyclohexane (1 volume

실험 절차

The procedure of Example 1 is followed using 6-t-butyl-3-(2-ethylhexylaminomethyl)-2,4-dimethylphenol (13.40 grams; 0.042 mole) and 1,3-benzenedisulfonyl chloride (5.5 grams; 0.02 mole) in a mixture of acetone (100 mls) and water (35 mls) while adding a solution of sodium hydroxide (1.76 grams; 0.044 mole) in water (15 mls) and maintaining the temperature at 30°-35° C. The mixture is allowed to stand at ambient temperature for 15 hours. After separating the oily layer, treating the same with ice water to effect crystallization, the solid is filtered to obtain the crude product (15.5 grams; 92% of theoretical). Recrystallization of the crude product from a mixture of benzene and cyclohexane (1 volume: 2 volumes, respectively) affords the desired product (5.5 grams; m.p. 135°-136° C.).

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