(2-AMINO-4,5,6,7-TETRAHYDRO-BENZO[B]THIOPHEN-3-YL)-PHENYL-METHANONE synthesis

Yield:4651-72-3 98%

Reaction Conditions:

with morpholine;sulfur in ethanol at 40;

Steps:

11.a

To a stirred solution of 0.60 g (4.13 mmol) 3-oxo-3-phenyl-propionitrile in 20 ml ethanol was added 0.43 ml (4.13 mmol) cyclohexanone, 133 mg (4.13 mmol) sulfur, and 0.36 ml (4.13 mmol) morpholine. The mixture was heated at 40 ⁰C over the night and then poured onto water and extracted three times with ethyl acetate. The combined organic phases were dried over sodium sulfate and concentrated in vacuo. Trituration in ether afforded 1.041 g (98%) (2-Amino-4,5,6,7-tetrahydro-benzo[b]thiophen-3-yl)-phenyl- methanone as an orange solid. ES-MS m/e (%): 258 (M+H+, 100).

References:

WO2006/63732,2006,A1 Location in patent:Page/Page column 27