Water → 4-[10-Oxo-9-(2,2,2-trifluoroethylcarbamoyl)-9,10-dihydro-10lambda4-thioxanthen-9-yl]butyl bromide

Temperature

0 °C

The compound (46 mg) prepared in step (d) of Example 133 was dissolved in dichloromethane (1 ml). m-Chloroperbenzoic acid (19 mg) was added to the solution at 0° C., and the mixture was stirred at 0° C. for one hr. Water was added to the reaction solution, and the mixture was extracted with chloroform. The extract was dried over anhydrous MgSO4, and the solvent was then removed by distillation under the reduced pressure. The residue was purified by preparative TLC (n-hexane:ethyl acetate=1:4) to give 4-[10-oxo-9-(2,2,2-trifluoroethylcarbamoyl)-9,10-dihydro-10λ4-thioxanthen-9-yl]butyl bromide (38 mg).

1. extractionthe mixture was extracted with chloroform
2. dry with materialThe extract was dried over anhydrous MgSO4
3. customthe solvent was then removed by distillation under the reduced pressure
4. customThe residue was purified by preparative TLC (n-hexane:ethyl acetate=1:4)

ORD record

ord-2afbded9a8f54ba9aca990363cbc83fe

Source dataset

uspto-grants-2004_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06777414B1