反应详情

Methyl 3-(2,5-dimethyl-1H-pyrrol-1-yl)-6-methoxy-5-(trifluoromethyl)picolinate (100 mg, 0.305 mmol) in acetonitrile (3.05 ml) was treated with KI (202 mg, 1.218 mmol) and TMS-Chloride (0.156 ml, 1.221 mmol) and heated at reflux for 6 hours. The solvent removed was in vacuo and the crude product was dissolved in EtOAc (20 ml) and washed with water (2×10 ml) and brine (10 ml), dried over a phase separator and concentrated in vacuo. Purification of the crude product by chromatography on silica eluting with iso-hexane: EtOAc (gradient of 0 to 30% EtOAc) afforded the title compound as an yellow powder. LC-MS Rt=1.11 mins [M+H]+ 315.4 (Method 2minLC_v003).

1. temperatureheated
2. temperatureat reflux for 6 hours
3. customThe solvent removed
4. dissolutionthe crude product was dissolved in EtOAc (20 ml)
5. washwashed with water (2×10 ml) and brine (10 ml)
6. customdried over a phase separator
7. concentrationconcentrated in vacuo
8. customPurification of the crude product by chromatography on silica eluting with iso-hexane