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85175-85-5

8-METHOXY-1,3-DIHYDRO-2H-3-BENZAZEPIN-2-ONE synthesis

3synthesis methods
-

Yield:85175-85-5 53%

Reaction Conditions:

with hydrogenchloride in water;acetic acid at 20;

Steps:

(c). 8-Methoxy-1,3-dihydrobenzo[d]azepine-2-one (2)

A solution of compound 1 (19.0 g, 75.0 mmol) in AcOH (54 mL) was added with stirring to concentrated HCl (36 mL). The mixture was stirred at rt overnight and poured into crushed ice. The precipitate was filtered. The filter cake was dissolved in CH2Cl2 which was washed with water and brine, dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The crude product was triturated with Et2O and filtered to afford 2 (7.45 g, 53%) as a white solid

References:

Wang, Min;Gao, Mingzhang;Steele, Brandon L.;Glick-Wilson, Barbara E.;Brown-Proctor, Clive;Shekhar, Anantha;Hutchins, Gary D.;Zheng, Qi-Huang [Bioorganic and Medicinal Chemistry Letters,2012,vol. 22,# 14,p. 4713 - 4718] Location in patent:experimental part

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