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 MgSO41 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. customThe extract was dried over anhydrous MgSO41
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-e7b0c53d875c46b793cb5fcca70cf6f1

Source dataset

uspto-grants-2006_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07030120B2