반응 #1243626

반응 방정식

( V )

4-methylcatechol

dibromomethane

( V )

4-methylcatechol

→

3,4-methylenedioxytoluene

수율 89.0%

용매

water

water

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise to a solution
2. 2
   온도under reflux condition
3. 3
   workup.ADDITIONAfter completion of the dropwise addition
4. 4
   온도the mixture was maintained at the same temperature for 2 hours
5. 5
   기타After completion of the reaction
6. 6
   추출the reaction mixture was extracted with toluene
7. 7
   기타after liquid separation
8. 8
   workup.DISTILLATIONthe toluene was distilled off from the resulting organic layer
9. 9
   workup.DISTILLATIONDistillation of the residue

실험 절차

Alternatively, a solution composed of 0.7 mol of the compound (V) obtained by the above process, 1.75 mols of sodium hydroxide, and a 2.8-fold amount by weight, based on (V), of water was added dropwise to a solution composed of a 1.6-fold amount by weight, based on (V), of water, 2.0 mols of dibromomethane, and 0.007 mol of tetra-n-butylammonium bromide over 5 hours under reflux condition. After completion of the dropwise addition, the mixture was maintained at the same temperature for 2 hours while stirring. After completion of the reaction, the reaction mixture was extracted with toluene and, after liquid separation, the toluene was distilled off from the resulting organic layer. Distillation of the residue gave 3,4-methylenedioxytoluene (VI-1) in 89% yield.

출처