反应详情

温度

100 °C

was prepared by use of 2,2,-trifluoro-1-methoxy-ethanol in place of chloral in the general method set forth above with the following procedural changes: A mixture of 4-bromobenzamide (0.78 g, 3.9 mmol) and 2,2,2-trifluoro-1-methoxy-ethanol (0.51 mL, 4.3 mmol) was heated at 100° C. for 18 hours. The mixture was evaporated and the residue was diluted with chloroform and concentrated onto silica gel. The product was purified on a SiO2 MPLC column with 1% MeOH:CH2Cl2 to yield the intermediate 4-bromo-N-(2,2,2-trifluoro-1-hydroxyethyl)benzamide, which was used in the general method set forth above to prepare Compound 13.

1. customThe mixture was evaporated
2. additionthe residue was diluted with chloroform
3. concentrationconcentrated onto silica gel
4. customThe product was purified on a SiO2 MPLC column with 1% MeOH