反应详情

To a stirred solution of N-(1-adamantylmethyl)-5-chloro-2-(3-hydroxypropyl)isonicotinamide (0.12 g, 0.33 mmol) (Example 14(ii)) in dry dichloromethane (10 mL) Dess-Martin periodinane (0.14 g, 0.33 mmol) was added. The resulting mixture was stirred at room temperature for 4 hours. The reaction was treated with diethyl ether (20 mL) and a saturated sodium bicarbonate solution containing sodium thiosulfate (0.37 g, in 4 mL). The mixture was stirred for 10 minutes and the organics separated; washed with brine (10 mL); dried over anhydrous magnesium sulfate; filtered; treated with acetic acid (0.30 mL) and concentrated. MS: APCI(+ve) 361, 363 (M+1).

1. stirringThe mixture was stirred for 10 minutes
2. washwashed with brine (10 mL)
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. additiontreated with acetic acid (0.30 mL)
6. concentrationconcentrated