2-Amino-6-fluoro-4-methoxy-benzonitrile synthesis
- Product Name:2-Amino-6-fluoro-4-methoxy-benzonitrile
- CAS Number:601517-02-6
- Molecular formula:C8H7FN2O
- Molecular Weight:166.15
123843-66-3
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Yield:601517-02-6 91%
Reaction Conditions:
with dihexyl phthalate;ammonia in dimethyl sulfoxide at 80;Sealed tube;
Steps:
51.4; 52.4 Step 4: 2-amino-6-fluoro-4-methoxybenzonitrile
To a solution of 2, 6-difluoro-4-methoxybenzonitrile (45 g, 266.3 mmol) in DMSO (400 mL) was added DHP (1.0 mL, 12.40 mmol) . Then ammonia was bubbled through the reaction mixture about 10 min and then the reaction mixture was sealed. After stirred at 80 overnight, the reaction mixture was diluted with water (300 mL) and extracted with EtOAc (300 mL x3) . The combined organic layer was washed with water (300 mL x3) and brine (300 mL) , dried over anhydrous Na 2SO 4, filtered and concentrated to give a residue. The residue was purified by silica gel chromatography (PE/EtOAc = 1/3) to give the product (40 g, 91%yield) as a white solid. MS (ESI) m/z: 167.1 (M+H) +.
References:
WO2020/57511,2020,A1 Location in patent:Page/Page column 176; 178
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