Some common heterocyclic compound, 18595-12-5, name is Methyl 5-amino-2-methylbenzoate, molecular formula is C9H11NO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. COA of Formula: C9H11NO2
4.6 g (28 mmol) of methyl 3-amino-6-methylbenzoate are dissolved in 50 ml of THF and 50 ml of 1M sulphuric acid and then the reaction medium is cooled to 0 C. A solution of sodium nitrite (2.3 g, 33.6 mmol) in 10 ml of water is then added dropwise and then the medium is stirred for 20 minutes. 15 ml of pure sulphuric acid are then added and the reaction medium is heated under reflux for 2 hours, poured into 500 ml of water and extracted with ethyl ether. The organic phases are dried, concentrated under reduced pressure and the residue obtained is dissolved in 100 ml of methanol. 3 ml of sulphuric acid are added and the reaction medium is heated under reflux for 14 hours, cooled, treated with water and ethyl ether. After extraction with ethyl ether, the organic phases are combined, dried over magnesium sulphate and concentrated under reduced pressure. After purification on a silica column (ethyl acetate 30-heptane 70), a brown oil is obtained (m=1.2 g; Y=25%).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 18595-12-5, its application will become more common.
Reference:
Patent; Galderma Research & Development S.N.C.; US6689922; (2004); B1;,
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