반응 #77961

반응 방정식

tert-butyl nitrite

dimethyl disulfide

4-bromo-2,3-dimethylaniline

→

2,3-dimethyl-4-methylthiobromobenzene

반응 조건

후처리

1. 1
   온도For work-up, the mixture is cooled
2. 2
   여과the residue is filtered off
3. 3
   세척the filtrate is washed with saturated aqueous NaHCO3 solution
4. 4
   기타For purification of the product
5. 5
   기타the organic phase is separated by distillation
6. 6
   기타Initially, the excess dimethyl disulfide is separated off at atmospheric pressure
7. 7
   기타1870 g of dimethyl disulfide (purity >97% according to GC) are recovered
8. 8
   workup.DISTILLATIONThe residue is subsequently subjected to fractional distillation under reduced pressure (0.1 mbar)

실험 절차

603 g (5.85 mol) of tert-butyl nitrite and 375 g of copper powder (5.9 mol) are initially charged in 3000 ml of dimethyl disulfide, and 761 g (3.75 mol) of 4-bromo-2,3-dimethylaniline are added dropwise at from 50 to 58° C. The mixture is subsequently stirred at from 75 to 80° C. for 9 hours. For work-up, the mixture is cooled, the residue is filtered off and the filtrate is washed with saturated aqueous NaHCO3 solution. For purification of the product, the organic phase is separated by distillation. Initially, the excess dimethyl disulfide is separated off at atmospheric pressure. 1870 g of dimethyl disulfide (purity >97% according to GC) are recovered. The residue is subsequently subjected to fractional distillation under reduced pressure (0.1 mbar).

출처