反应详情

2-Chloro-4-[4-(trifluoromethyl)phenyl]pyrimidine (which may be prepared as described in Description 5) (1.22 g, 4.72 mmol) was added portionwise to HI (57% in water) (4.98 mL, 37.74 mmol) at 0° C. and the dark mixture was stirred for 40 mins. Dichloromethane (5 mL) was added and the resultant light brown mixture was stirred at 0° C. for 18.25 hrs. Additional dichloromethane (5 mL) was added followed by HI (57% in water) (1.87 mL, 14.15 mmol) and vigorous stirring was continued at 0° C. for a further 18 hrs. The mixture was quenched by the addition of satd. aq. K2CO3 (care: gas evolved). After basification, satd. 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 the 2-iodo-4-[4-(trifluoromethyl)phenyl]pyrimidine (D6) (1.57 g, 4.48 mmol, 95.1% yield) as a yellow solid.

1. stirringthe resultant light brown mixture was stirred at 0° C. for 18.25 hrs
2. stirringvigorous stirring
3. waitwas continued at 0° C. for a further 18 hrs
4. customThe mixture was quenched by the addition of satd
5. additionsodium metabisulphite was added
6. stirringstirring
7. waitwas continued for 5 mins
8. additionThe mixture was diluted with further DCM
9. customthe phases were separated
10. dry with materialThe organic layer was dried (Na2SO4)
11. customthe solvent evaporated