5-Bromo-2-chloro-3-(difluoromethyl)pyridine synthesis
- Product Name:5-Bromo-2-chloro-3-(difluoromethyl)pyridine
- CAS Number:1332392-76-3
- Molecular formula:C6H3BrClF2N
- Molecular Weight:242.45
228251-24-9
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1332392-76-3
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$180.00/1g
Yield:1332392-76-3 87%
Reaction Conditions:
with diethylamino-sulfur trifluoride in ethanol;dichloromethane at 25; for 2.25 h;
Steps:
58.2 Step-2: 5-bromo-2-chloro-3-(difluoromethyl)pyridine:
To a solution of step-1 intermediate (4.79 g, 21.73 mmol) in DCM (125 mL) was added catalytic amount of ethanol (0.127 mL, 2.173 mmol) followed by the addition of DAST (5.74 mL, 43.5 mmol) dropwise at 25eC for 15 min. Reaction mixture was stirred at same temperature for 2h before quenching with aqueous saturated solution of NaHCC at OeC. The layers were separated and the aqueous layer was washed with DCM. Combined organic layer was washed with brine, dried over Na2SC>4 and concentrated in vaccum and the crude product was purified by flash column chromatography (silica gel) to afford 4.60 g (87%) of the titled compound. 1HNMR (400 MHz, DMSO-d6) ||8.79 (d, J = 2.5 Hz, 1H), 8.42 (d, J = 2.5 Hz, 1H), 7.21 (t, J = 53.5 Hz, 1H); GCMS (m/z) 240.85 (M)+.
References:
WO2018/20474,2018,A1 Location in patent:Page/Page column 157
78686-79-0
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1332392-76-3
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$180.00/1g
742100-75-0
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1332392-76-3
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$180.00/1g