5-NITROTHIOPHENE-2-CARBOXYLICMETHYLESTER synthesis
- Product Name:5-NITROTHIOPHENE-2-CARBOXYLICMETHYLESTER
- CAS Number:5832-01-9
- Molecular formula:C6H5NO4S
- Molecular Weight:187.17
Yield:5832-01-9 96.5%
Reaction Conditions:
with iodine;sodium hydrogencarbonate in methanol;n-heptane;
Steps:
3 Preparation of methyl 5-nitro-2-thenoate
EXAMPLE 3 Preparation of methyl 5-nitro-2-thenoate Into a 250-ml flask fitted with a central stirrer, a thermometer and a condenser and containing 15.7 g (0.1 mol) of 5-nitro-2-formylthiophene, were introduced 21 g (0.25 mol) of sodium bicarbonate and 100 ml of pure methanol. By small portions, 30.5 g (0.12 mol) of iodine were adeed to the reaction medium at the temperature of 0° C. The operation of addition lasted one hour. After that, the medium was maintained at the reflux temperature of the methanol for 2 hours until it became totally discoloured and then it was poured into water and extracted with ethyl ether. The ethereal phase was washed with water, dried on sodium sulphate and heated to dryness in a rotatory evaporator. The crude solid so obtained was recristallized from a 70/30 heptane/1,2-dichloro-ethane mixture and then brought to 0° C. In this manner, 18 g of crude methyl 5-nitro-2-thenoate were obtained which represents a yield of 96.5%. M.P.: 74° C.
References:
US4219482,1980,A
4521-33-9
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5832-01-9
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$6.00/1g
