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
99368-66-8
210 suppliers
$5.00/250mg
99368-67-9
135 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
680-15-9
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$13.00/5g
25391-60-0
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$27.00/100mg
99368-67-9
135 suppliers
$7.00/250mg
99368-66-8
210 suppliers
$5.00/250mg
99368-67-9
135 suppliers
$7.00/250mg
22245-83-6
305 suppliers
$6.00/5g
99368-67-9
135 suppliers
$7.00/250mg
65753-47-1
380 suppliers
$8.00/5g
99368-67-9
135 suppliers
$7.00/250mg