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2-CHLORO-5-NITRO-3-(TRIFLUOROMETHYL)PYRIDINE synthesis
- Product Name:2-CHLORO-5-NITRO-3-(TRIFLUOROMETHYL)PYRIDINE
- CAS Number:99368-67-9
- Molecular formula:C6H2ClF3N2O2
- Molecular Weight:226.54
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99368-66-8
207 suppliers
$5.00/250mg
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99368-67-9
136 suppliers
$7.00/250mg
Yield:99368-67-9 86%
Reaction Conditions:
with thionyl chloride in N,N-dimethyl-formamide at 100; for 10 h;Temperature;
Steps:
8.2 2-Chloro-5-nitro-3-(trifluoromethyl)pyridine
SOCl2 (18.45 mL, 253 mmol) was added to a solution of 5-nitro-3-(trifluoromethyl)pyridin-2-ol (2.63 g, 12.64 mmol). DMF (1.957 mL, 25.3 mmol) was added and the mixture was at 100° C. for 10 h. Then the solution was concentrated and distributed between EA and saturated NaHCO3 solution. The combined organic extract was washed with brine, dried over MgSO4, filtered and concentrated. The resulting 2-chloro-5-nitro-3-(trifluoromethyl)pyridine (2.46 g, 10.86 mmol, 86% yield) was used in the next step without further purification. TLC (PE/EA=5:1, Rf=0.6): 1H NMR (400 MHz, CDCl3) δ: 9.23-9.59 (m, 1H), 8.79 (d, J=2.4 Hz, 1H).
References:
GlaxoSmithKline Intellectual Property Development Limited;EIDAM, Hilary Schenck;Raha, Kaushik;Gong, Zhen;Guan, Huiping;Wu, Chengde;Yang, Haiying;Yu, Haiyu;Zhang, Zhiliu;CHEUNG, Mui US2014/275111, 2014, A1 Location in patent:Paragraph 0259; 0260
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680-15-9
249 suppliers
$13.00/5g
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25391-60-0
51 suppliers
$27.00/100mg
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99368-67-9
136 suppliers
$7.00/250mg
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99368-66-8
207 suppliers
$5.00/250mg
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99368-67-9
136 suppliers
$7.00/250mg

22245-83-6
300 suppliers
$6.00/5g
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99368-67-9
136 suppliers
$7.00/250mg
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65753-47-1
375 suppliers
$8.00/5g
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99368-67-9
136 suppliers
$7.00/250mg