반응 #77962

반응 방정식

tert-butyl nitrite

dimethyl disulfide

2,3-dimethylaniline

dimethyl disulfide

→

2,3-dimethylthioanisole

반응 조건

후처리

1. 1
   온도For work-up, the mixture is cooled
2. 2
   여과filtered off with suction through kieselguhr
3. 3
   세척the filtrate is washed with saturated aqueous NaHCO3 solution
4. 4
   기타For the purification of the product
5. 5
   기타the organic phase is separated by distillation
6. 6
   기타Initially, excess dimethyl disulfide is removed at atmospheric pressure
7. 7
   기타1446 g of dimethyl disulfide (purity>97% according to GC) are recovered
8. 8
   workup.DISTILLATIONThe residue is then subjected to fractional distillation under reduced pressure (0.1 mbar)

실험 절차

355 g (3.44 mol) of tert-butyl nitrite and 250 g of copper powder (3.9 mol) are initially charged in 1250 ml of dimethyl disulfide, and a solution of 250 g (2.07 mol) of 2,3-dimethylaniline in 1000 ml of dimethyl disulfide is added dropwise at 50-52° C. The mixture is subsequently stirred at 75-80° C. for 1.5 hours. For work-up, the mixture is cooled, filtered off with suction through kieselguhr, and the filtrate is washed with saturated aqueous NaHCO3 solution. For the purification of the product, the organic phase is separated by distillation. Initially, excess dimethyl disulfide is removed at atmospheric pressure. 1446 g of dimethyl disulfide (purity>97% according to GC) are recovered. The residue is then subjected to fractional distillation under reduced pressure (0.1 mbar).

출처