Methyl 5-Methyl-4-nitrothiophene-2-carboxylate synthesis
- Product Name:Methyl 5-Methyl-4-nitrothiophene-2-carboxylate
- CAS Number:56921-01-8
- Molecular formula:C7H7NO4S
- Molecular Weight:201.2
67-56-1
789 suppliers
$9.00/25ml
36050-35-8
37 suppliers
inquiry
56921-01-8
37 suppliers
$50.00/100mg
Yield:56921-01-8 98%
Reaction Conditions:
with sulfuric acid at 20;Heating / reflux;
Steps:
14.1
Fuming nitric acid (3 eq.) was added dropwise to Ac2O (5 eq.) at -200C, then 5-methyl-2- thiophenecarboxylic acid (1 eq.) was added portion-wise and the mixture placed in an ice bath. After stirring at 00C for 1.5 h the reaction mixture was poured into ice, and when the ice was molten the precipitate was filtered off (66%). To a IM solution of the latter in MeOH, cone. H2SO4 (1.4 eq.) was added at RT. The mixture was stirred overnight at reflux. All volatiles were evaporated i. vac, then the residual material was mixed with water and the resulting solution extracted with EtOAc; the organic layer was washed with sat. NaHCO3 and brine, dried over Na2SO4 and concentrated (98%). 1H-NMR (400 MHz, CDCl3, 300K, δ) 8.21 (IH, s), 3.93 (s, 3H), 2.85 (s, 3H).
References:
WO2006/119975,2006,A1 Location in patent:Page/Page column 37
19432-69-0
64 suppliers
$24.00/250mg
56921-01-8
37 suppliers
$50.00/100mg
24647-78-7
27 suppliers
inquiry
64-19-7
1618 suppliers
$10.00/25ML
56921-01-8
37 suppliers
$50.00/100mg
1918-79-2
246 suppliers
$8.00/5g
56921-01-8
37 suppliers
$50.00/100mg
5380-42-7
177 suppliers
$6.00/1g
56921-01-8
37 suppliers
$50.00/100mg