1-CHLORO-2-NITRO-4-TRIFLUOROMETHANESULFONYL-BENZENE synthesis
- Product Name:1-CHLORO-2-NITRO-4-TRIFLUOROMETHANESULFONYL-BENZENE
- CAS Number:1550-27-2
- Molecular formula:C7H3ClF3NO4S
- Molecular Weight:289.62
383-11-9
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1550-27-2
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$144.00/1 g
Yield:1550-27-2 24%
Reaction Conditions:
with sulfuric acid;sulfur trioxide;nitric acid at 100; for 24 h;
Steps:
276
To a stirred solution of compound 276.1 (500 mg, 0.002049 mol), in Oleum (2.5 g, 0.014 mol) was added fuming HNO3 (5 ml). The resulting reaction mixture was stirred at 100 °C for 24 hr. After completion of the starting material (by TLC), the reaction mixture was quenched with water (10 ml) and the extracted o was extracted with CH2Cl2 (2x10 ml). The organic layer was washed with water (20 ml) and dried over anhydrous sodium sulphate and evaporated under reduced pressure. The crude material was purified by column chromatography [silica gel (60-120 mesh, 4Og), 30 mm diameter, 500 mm length gradient (5-15% EtOAc/Hexane)] to afford compound 276.2 (2 g, 24%) as colorless liquid. 1H-NMR (CDCl3, 500 MHz) δ 8.53 (bs, 1H), 8.19-8.14 (m, 1H), 7.94 (d, J = 8.8 Hz, 1H).
References:
BIOGEN IDEC MA INC.;SUNESIS PHARMACEUTICALS, INC.;CHUAQUI, Claudio;COSSROW, Jennifer;DOWLING, James;GUAN, Bing;HOEMANN, Michael;ISHCHENKO, Alexey;JONES, John, Howard;KABIGTING, Lori;KUMARAVEL, Gnanasambandam;PENG, Hairuo;POWELL, Noel;RAIMUNDO, Brian;TANAKA, Hiroko;VAN VLOTEN, Kurt;VESSELS, Jeffrey;XIN, Zhili WO2010/78408, 2010, A1 Location in patent:Page/Page column 161; 162
407-16-9
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$39.00/500 mg
1550-27-2
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$144.00/1 g
706-29-6
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1550-27-2
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$144.00/1 g
123-09-1
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$17.00/25g
1550-27-2
30 suppliers
$144.00/1 g