反应详情

Hydroiodic acid (57% in water, 9.68 mL, 73.41 mmol) was added portionwise to 2-chloro-4-methyl-6-[4-(trifluoromethyl)phenyl]pyrimidine (which may be prepared as described in Description 5) (1.38 g, 5.06 mmol) in DCM (30 mL) at 20° C. and the dark mixture was stirred for 18 hrs. The mixture was quenched by the addition of sat. aq. K2CO3 (care: gas evolved). After basification, satd. aq. sodium metabisulphite was added and stirring was continued for 5 mins. The mixture was diluted with further DCM and the phases were separated. The organic layer was dried (Na2SO4) and the solvent evaporated to afford 2-iodo-4-methyl-6-[4-(trifluoromethyl)phenyl]pyrimidine (D6) (1.58 g, 4.34 mmol, 85.7% yield) a yellow solid, containing about 20% of the reduced H-compound.

1. customThe mixture was quenched by the addition of sat. aq. K2CO3 (care: gas evolved)
2. additionaq. sodium metabisulphite was added
3. stirringstirring
4. waitwas continued for 5 mins
5. additionThe mixture was diluted with further DCM
6. customthe phases were separated
7. dry with materialThe organic layer was dried (Na2SO4)
8. customthe solvent evaporated