N-(5-Bromo-4-methoxy-2-nitrophenyl)acetamide synthesis
- Product Name:N-(5-Bromo-4-methoxy-2-nitrophenyl)acetamide
- CAS Number:7357-66-6
- Molecular formula:C9H9BrN2O4
- Molecular Weight:289.08
6943-73-3
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7357-66-6
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Yield:7357-66-6 97%
Reaction Conditions:
with HNO3 in acetic anhydride at -10 - -5; for 1 h;
Steps:
223.223B Example 223; 3-[(3,5-difluorophenyl)amino]-7-(3-hydroxy-3-methylbutyl)-8-methoxy-5,10-dihydro-11H-dibenzo[b,e][1,4]diazepin-11-one; Example 223B; N-(5-bromo-4-methoxy-2-nitrophenyl)acetamide
Concentrated nitric acid (10 ML, >69% pure) was added to acetic anhydride (50 mL) cooled TO-10 C. The solution was treated portionwise with Example 223A (5.08 g, 20.8 mmol) at a rate which maintained an internal temperature BELOW-5 C. The solution was stirred for 1 hour while warming to room temperature. The solution was poured into an ice/water mixture and extracted several times with ethyl acetate. The combined extracts were washed with 10% NA2CO3 and brine, dried (MGS04), filtered, and concentrated under vacuum. The residue was purified by flash column chromatography on silica gel with 3: 7 hexanes/ethyl acetate to provide 5.88 g (97%) of the title compound. MS (DCI) m/e 290 (M+H) + ; 1H NMR (500 MHz, DMSO- D6) 8 10. 11 (S, 1H), 7.87 (s, 1H), 7.61 (s, 1H), 3.93 (s, 3H), 2.04 (s, 3H).
References:
WO2004/76424,2004,A1 Location in patent:Page 144
19056-41-8
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108-24-7
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7357-66-6
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$145.00/500mg
51-66-1
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7357-66-6
23 suppliers
$145.00/500mg