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4-(4-Amino-2-methylphenyl)morpholin-3-one synthesis

3synthesis methods
4-(2-Methyl-4-nitrophenyl)morpholin-3-one

845729-40-0
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4-(4-Amino-2-methylphenyl)morpholin-3-one

482308-10-1
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Yield:482308-10-1 97%

Reaction Conditions:

with hydrogen;Raney nickel in methanol at 20; under 3750.38 Torr; for 2 h;

Steps:

1.c (c)

(c) 3-methyl-4-(3-oxo-morpholin-4-yl)-aniline 770 mg (3.26 mmol) 3-methyl-1-nitro-4-(3-oxo-morpholin-4-yl)-benzene are hydrogenated in a Parr apparatus in 50 ml of methanol together with 100 mg Raney nickel under a hydrogen atmosphere at 5 bars pressure at ambient temperature for 2 h. After filtration the mixture is evaporated down i. vac., the residue is combined in each case with ethanol and dichloromethane and evaporated down completely. The residue is further reacted without any further purification. Yield: 650 mg (97%) Rf value: 0.31 (silica gel; ethyl acetate+0.5% conc. ammonia solution) C11H14N2O2 (206.24) Mass spectrum: (M+H)+=207

References:

US2008/51578,2008,A1 Location in patent:Page/Page column 31-32