Category: 13101-88-7

Application of 13101-88-7,Some common heterocyclic compound, 13101-88-7, name is 6-Methoxynaphthalen-2-amine, molecular formula is C11H11NO, 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.

28.2 g (0.16 mol) of the product synthesised in the previous step are dissolved in a mixture of dichloromethane/methanol: 1500/620 ml. To the resulting solution add, at ambient temperature, 56.7 g (0.16 mol) of benzyltrimethylammonium dichloroiodate and 21.2 g (0.212 mol) of calcium carbonate. After 30 minutes, filter off the insoluble material, then take up the organic phase with 10% sodium bisulphite solution and extract with ethyl ether. Dry over magnesium sulphate, filter and then evaporate. The residue is purified by chromatography over silica gel using a mixture of cyclohexane/ethyl acetate:70/30:v/v as eluant.

The synthetic route of 13101-88-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Lavielle, Gilbert; Muller, Olivier; Millan, Mark; Gobert, Alain; Di Cara, Benjamin; US2005/59675; (2005); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 13101-88-7, name is 6-Methoxynaphthalen-2-amine, A new synthetic method of this compound is introduced below., Quality Control of 6-Methoxynaphthalen-2-amine

Weigh compound 6-methoxy-2-naphthyl-amine (7g, 0.04044mol), triethylamine (6g, 0.06067mol) in 100mL reaction flask, a solution of methylene chloride was added to the reaction flask of 15mL at 0 the reaction conditions under 15min; dropwise added methanesulfonyl chloride (7g, 0.06067mol), under reaction conditions 0 30min, TLC plate monitor, the reaction was complete, adding an appropriate amount of aqueous sodium hydroxide solution, extracted with ethyl acetate and saturated brine dried over anhydrous sodium sulfate, and spin dry, column chromatography (PE: EA = 2: 1), give a purple solid 5.6g, yield 55.2%.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; East China University of Science and Technology; Li, Hongling; Jiang, Hualiang; Xu, Yufang; Li, Jia; Zhao, Zhenjang; Li, Jingya; Xu, Hongling; Li, Shiliang; (64 pag.)CN105566276; (2016); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Application of 13101-88-7, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 13101-88-7 as follows.

1.- 2,5-dimethyl-2-(6-methoxynaphthalen-2-yldiazenyl)furan-3(2H)-one To a suspension of 2-amino-6-methoxynaphthalene (2.6 g, 15 mmol) in H2O (40 ml), HCl conc. was added (8 ml), it was cooled in an ice bath and a NaNO2 solution (1.19 g, 17.3 mmol) in H2O (18 ml) was added dropwise shaking the mixture at 0?C during 30 minutes. The previous solution was diluted in H2O (80 ml), 2,5-dimethylfuran-2,3-dihydrofuran-3-one (1.94 g, 17.3 mmol) was added and was left shaking during 2 hrs at room temperature resulting in a yellow precipitate. It was filtered, washed with water and dried. It was thereby obtained 2,5-dimethyl-2-(6-methoxynaphthalen-2-yldiazenyl)furan-3-one (4.22 g, 95 %) in a solid crude form of an ocre-yellow color that was used directly in the following synthesis step. 1H-NMR (300 MHz, CDCl3) delta ppm: 8.35 (s, 1H), 7.85 (d, J=8,8Hz, 1H), 7.75-7.7 (m, 2H), 7.2 (m, 2H), 5.55 (s, 1H), 3.95 (s, 3H), 2.45 (s, 3H), 1.75 (s, 3H).

According to the analysis of related databases, 13101-88-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Laboratorios Del. Dr. Esteve, S.A.; EP2113501; (2009); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem