反应详情

温度

190 °C

A solution of (R)-N-[2-chloro-4-iodophenyl]-2-hydroxy-2-methyl-3,3,3-trifluoropropanamide (Example 197) (0.8 g) in pyridine (1 ml) was added to a deoxygenated solution of 2-mercaptoethanol (0.18 ml), sodium methoxide (0.14 g) and copper(I) chloride (0.2 g) in quinoline (2 ml) and pyridine (2 ml). The mixture was heated to 190° C. under argon for 18 hours. The mixture was allowed to cool to room temperature then dissolved in ethyl acetate (100 ml), washed with dilute aqueous hydrochloric acid (2×50 ml) and brine (2×50 ml) then dried. Volatile material was removed by evaporation and the residue was purified by chromatography on a silica gel Mega Bond Elut column eluting with 10-60% ethyl acetate/iso-hexane to give the title compound as a gum. NMR (CDCl3): 1.76 (s, 3H), 3.10 (t, 2H), 3.75-3.80 (m, 2H), 7.31-7.34 (m, 1H), 7.47 (s, 1H), 8.31 (d, 1H), 8.86 (s, 1H); MS (ESPF): 342.

1. temperatureto cool to room temperature
2. washwashed with dilute aqueous hydrochloric acid (2×50 ml) and brine (2×50 ml)
3. customthen dried
4. customVolatile material was removed by evaporation
5. customthe residue was purified by chromatography on a silica gel Mega Bond Elut column
6. washeluting with 10-60% ethyl acetate/iso-hexane