Benzoic acid, 4-amino-5-fluoro-2-methoxy-, methyl ester (9CI) synthesis
- Product Name:Benzoic acid, 4-amino-5-fluoro-2-methoxy-, methyl ester (9CI)
- CAS Number:617246-14-7
- Molecular formula:C9H10FNO3
- Molecular Weight:199.18
247071-37-0
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617246-14-7
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Yield:617246-14-7 17%
Reaction Conditions:
with hydrogenchloride in methanol;water at 40 - 70;
Steps:
109 Example 109; 4-Amino-5-fluoro-2-methoxy-benzoic acid methyl ester
To a saturated solution of gas hydrogen chloride in METHANOL (20ML) and water (0. 04MOI) was added Ex 108 (290mg, 1.74 MMOL). The reaction mixture was stirred overnight at 40°C and then at 70°C for 5 hours. Solvent was removed in vacuo. The residue was partitioned between sat. aq. NAHCO3 and DICHLOROMETHANE. The aqueous phase was extracted with DICHLOROMETHANE (2x). The organic phases were combined, washed with brine, dried over MGS04 and concentrated in vacuo. The crude was purified over silica gel chromatography (EtOAc/Heptane: 1/9 to 1/1) to give the title compound Ex 109 as a white solid (60 mg, 0.30 mmol, 17%). 1H-NMR (CDCI3) : 6 3.83 (s, 3H), 3.84 (s, 3H), 6.3 (d, 1H), 7.56 (d, 1H)
References:
WO2004/48319,2004,A1 Location in patent:Page 67
