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To a refluxed mixture of 4.63 M sodium methoxide in methanol (55.0 mL, 254 mmol) and methanol (500 mL) was added solid N-acethonylphthalimide (25.00 g, 123.0 mmol, from TCI) in one portion. After addition, the reaction was heated at reflux for 2 hours, then cooled at 0 C and neutralized with 1 N HCl. The resulting suspension was stirred at 0 C for 30 minutes and then filtered under reduced pressure, washed with a small amount of water and air dried. The resulting solid was further dried under vacuum, over P2O5, to give the desired product (21.2 g, 85%). LCMS calculated for CnHi0NO3 (M+H)+: m/z = 204.1; Found: 204.0.
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Reference:
Patent; INCYTE CORPORATION; LI, Yun-Long; COMBS, Andrew, P.; YUE, Eddy, W.; LI, Hui-Yin; WO2011/75630; (2011); A1;,
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