반응 #93446

반응 방정식

BF3

( a )

4-Methyl-4-(3,5-di-tert-butyl-4-hydroxyphenylthio)-2-pentanone

2,6-di-tert-butyl-4-mercaptophenol

→

4-Methyl-2,2,4-tris(3,5-di-tert-butyl-4-hydroxyphenylthio)pentane

용매

toluene

반응 조건

후처리

1. 1
   온도The mixture is heated at 55°-65° C. for nine hours and 105°-110° C. for three additional hours
2. 2
   세척The toluene solution is washed with water
3. 3
   건조dried over sodium sulfate
4. 4
   기타The residue, isolated by evaporation of the solvent by distillation in vacuum
5. 5
   기타is purified
6. 6
   온도on cooling

실험 절차

0.11 Grams of BF3 -etherate is added to a solution of 2.70 grams of the product from (a) and 4.14 grams of 2,6-di-tert-butyl-4-mercaptophenol dissolved in 30 ml of toluene. The mixture is heated at 55°-65° C. for nine hours and 105°-110° C. for three additional hours. The toluene solution is washed with water and dried over sodium sulfate. The residue, isolated by evaporation of the solvent by distillation in vacuum, is purified by passing a solution in 70:30 heptane:toluene through a flash chromatographic column using silica gel. The isolated residue solidifies on cooling, and melts at 93°-115° C.

출처