反应详情

温度

0 °C

To periodic acid (68 mg, 0.30 mmol) in CH3CN (200 μL) at 0° C., Cr(VI)oxide (0.7 mg, 0.0073 mmol) was added and the mixture was stirred for 15 min at 0° C. A solution of 4-chloro-3-(4-cyano-6-trifluoromethyl-pyridin-3-yl)-N-[2-(3-hydroxy-2,2-dimethyl-propoxy)-phenyl]-N-methyl-benzamide (29 mg, 0.056 mmol) dissolved in CH3CN (200 μL) was added and the mixture was warmed to rt. After 2 hr at rt, the mixture was filtered, rinsed with CH3CN, concentrated, dissolved in MeOH and purified by prep HPLC yielding 3-(2-{[4-chloro-3-(4-cyano-6-trifluoromethyl-pyridin-3-yl)-benzoyl]-methyl-amino}-phenoxy)-2,2-dimethyl-propionic acid 52-1. MS: 532.3 (M+H)+, tR=3.65 min (method 3).

1. additionwas added
2. temperaturethe mixture was warmed to rt
3. waitAfter 2 hr at rt
4. filtrationthe mixture was filtered
5. washrinsed with CH3CN
6. concentrationconcentrated
7. dissolutiondissolved in MeOH
8. custompurified by prep HPLC