反应详情

A solution of the product of example 2 step (iii) (0.34 g), 4-(dimethylamino)pyridine (0.34 g), 3-amino-5-trifluoromethyl-1,2,4-triazole (J. Gen. Chem. USSR (Engl. Transl.) 1983, vol53, part 7, p1514) (0.42 g) and N,N-diisopropylethylamine (1.46 ml) in N,N-dimethylformamide (6 ml) was treated with bromo-tris(pyrrolidino)phosphonium hexafluorophosphate (1.3 g). After 2 hours the solution was quenched with aqueous tartaric acid. The solution was extracted with ethyl acetate. The combined extracts were washed with brine, dried (MgSO4) and evaporated under reduced pressure. Purification was by chromatography eluting with 30% ethyl acetate in toluene. The product was triturated with ethyl acetate/isohexane and the solid collected.

1. customAfter 2 hours the solution was quenched with aqueous tartaric acid
2. extractionThe solution was extracted with ethyl acetate
3. washThe combined extracts were washed with brine
4. dry with materialdried (MgSO4)
5. customevaporated under reduced pressure
6. customPurification
7. washeluting with 30% ethyl acetate in toluene
8. customThe product was triturated with ethyl acetate/isohexane
9. customthe solid collected