反应详情

To a solution of diacid (Step 4) (360 mg) in dichloromethane (28 mL) and acetonitrile (7.1 mL) was added 2-chloro-1-methylpyridinium iodide (227 mg). The solution was cooled to 0 C. and triethylamine (123 μL) was added. After stirring for 15 min, 0.42 mL of a 2M solution of dimethylamine in toluene was added. The solution was stirred 1 hr at room temperature, washed with acidified 25% ammonium acetate, dried over sodium sulfate, filtered and evaporated to dryness. To the oil obtained after chromatography, in 2 mL of ethanol, was added 0.154 mL of 2N NaOH. After evaporating to dryness the title compound was obtained as a foam.

1. temperatureThe solution was cooled to 0 C
2. stirringThe solution was stirred 1 hr at room temperature
3. washwashed
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. customevaporated to dryness
7. customTo the oil obtained after chromatography
8. customAfter evaporating to dryness the title compound
9. customwas obtained as a foam