2-Chloro-4-methyl-5-nitropyridine synthesis
- Product Name:2-Chloro-4-methyl-5-nitropyridine
- CAS Number:23056-33-9
- Molecular formula:C6H5ClN2O2
- Molecular Weight:172.57
21901-41-7
288 suppliers
$6.00/1g
23056-33-9
345 suppliers
$3.00/1g
17288-53-8
102 suppliers
$14.00/100mg
Yield:17288-53-8 95%
Reaction Conditions:
with thionyl chloride in N-methyl-acetamide;dichloromethane;toluene;
Steps:
12 5-Methoxypyrrolo[2,3-c]pyridine (Compound 9)
EXAMPLE 12 5-Methoxypyrrolo[2,3-c]pyridine (Compound 9) A mixture of 4-methyl-5-nitro-1H-pyridine-2-one (5.00 g, 32.44 mmol), thionyl chloride (20 ml), and two drops of dimethylformamide was heated atreflux under nitrogen for 52 hours. The resultant orange colored solution was evaporated under reduced pressure, and a small amount of anhydrous toluene was added and then removed via evaporation under reduced pressure to remove traces of thionyl chloride. The residual oil then passed througha silica gel filter (dried at 150° C. under vacuum overnight, approximately 100 g) followed by methylene chloride (1 1). This filtrate was evaporated under reduced pressure to afford 2-chloro-4-methyl-5-nitropyridine (5.30 g, 30.71 mmol, 95%) as an orange oil, which crystallized below 0° C.; IR (CHCl3) 1605, 1550, 1520, 1450, 1360, 1345 cm-1; 1 H NMR (CDCl3) δ 9.03 (s, 1H), 7.83 (s, 1H), 2.60 (s, 3H); LRMS (m/z, relative intensity) 174 (25), 173 (19), 172 (M+, 68), 157 (74), 155 (100), 128 (27), 101 (47), 100(55], 99 (74), 90 (43), 75 (36).
References:
US5051412,1991,A
21901-41-7
288 suppliers
$6.00/1g
23056-33-9
345 suppliers
$3.00/1g
21901-40-6
301 suppliers
$6.00/1g
23056-33-9
345 suppliers
$3.00/1g
695-34-1
546 suppliers
$5.00/10g
23056-33-9
345 suppliers
$3.00/1g
695-34-1
546 suppliers
$5.00/10g
23056-33-9
345 suppliers
$3.00/1g
23056-39-5
333 suppliers
$6.00/1g