反应详情

Dissolve (R)-1-benzoyl-3-(1-methyl-2,2,2-trifluoroethyl)-thiourea (6.2 g, 22.5 mmol) in methanol and add a solution of potassium carbonate (13.8 g, 100 mmol) in water (30 mL). Stir vigorously at room temperature overnight. Evaporate to dryness, dissolve residue in hot water (ca. 100 mL) and filter the resulting white crystals. Cool filtrate to 0° C., seed with crystals from hot water filtration, filter and collect resulting white crystals to obtain the desired intermediate (2.9 g, 74%). MS (ES+) m/z: 173 (M+H)+.

1. customEvaporate to dryness
2. dissolutiondissolve residue in hot water (ca. 100 mL)
3. filtrationfilter the resulting white crystals
4. filtrationCool filtrate to 0° C., seed with crystals from hot water filtration
5. filtrationfilter
6. customcollect
7. customresulting white crystals