Trifluoroacetic anhydride → HCID 54333950, compound

Trifluoroacetic anhydride (5 ml) was added to (R)-N-(2-chloro-4-methylsulphinyl-phenyl)-2-hydroxy-2-methyl-3,3,3-trifluoropropanamide (Example 92) (0.188 g). The mixture was stirred and heated under reflux for 45 minutes then cooled and evaporated to dryness. A mixture of triethylamine (5 ml) and methanol (5 ml) was added to the residue. This mixture was stirred for a further 45 minutes then evaporated to dryness. The residue was dissolved in chloroform (50 ml), washed with saturated aqueous ammonium chloride solution (50 ml), dried and concentrated by evaporation to give the title compound (0.177 g) as a gum which was used without purification. MS (ESP−): 298.

1. temperatureheated
2. temperatureunder reflux for 45 minutes
3. temperaturethen cooled
4. customevaporated to dryness
5. additionA mixture of triethylamine (5 ml) and methanol (5 ml)
6. additionwas added to the residue
7. stirringThis mixture was stirred for a further 45 minutes
8. customthen evaporated to dryness
9. dissolutionThe residue was dissolved in chloroform (50 ml)
10. washwashed with saturated aqueous ammonium chloride solution (50 ml)
11. customdried
12. concentrationconcentrated by evaporation

ORD record

ord-0d2a27b884064e1d87d0556f83c549b7

Source dataset

uspto-grants-2002_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06498275B1