Category: 4093-31-6

Related Products of 4093-31-6, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 4093-31-6, name is Methyl 4-acetamido-5-chloro-2-methoxybenzoate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A stirred suspension of methyl 4-(acetylamino)-5-chloro-2- (methyloxy)benzoate (103g, 0.4mol) in dry DCM (460ml) was cooled to 00C under argon. A solution of BCI3 in DCM (1 M) (800ml) was then cannulated directly from the reagent bottle with argon pressure by T-piece bleed control so that the rate of addition was easily controlled. The apparatus was set to control the internal temperature at 00C during the addition. The addition was carried out over 55 minutes. The temperature range (internally) varied 0?11C. During the addition the apparatus was kept under argon only by the supply of BCI3 through argon pressure. The vessel was capped with a silica drying tube. The suspension was present throughout the addition – it did not dissolve at any stage. After the complete addition of the BCI3 solution the temperature was adjusted to 15C and stirred for 1.5 hours under argon. After 1.5 hours under argon the mixture was poured into water (1 L), ice (35Og) with stirring and more DCM (0.8L) and water (0.8L) was added to this mixture. The whole mixture was transferred to a 5L separating funnel and vigorously shaken (solids virtually dissolved). Layers were separated and the aqueous layer extracted with DCM (2x 0.8L). The combined organic extracts were dried (MgSO4) and combined with the same extract obtained from repeating the above-mentioned reaction using the same reactant quantities. The combined extracts from the two experiments were concentrated in vacuo to a cream solid. This solid was stirred with Et2O (800ml) for 10 minutes. Then hexane (800ml) was added and the reaction continued to stir at room temperature for 0.5 hours. The solid was then filtered and washed with hexane (2 x 300ml) and dried at 45C under vacuum for 16 hours (185g, 0.759mol, 95%th) and identified as pure product. LCMS RT 2.44 mins (MH+)HPLC -99% (RT 11.9 min) at 254nm detection

The synthetic route of Methyl 4-acetamido-5-chloro-2-methoxybenzoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2007/96352; (2007); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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 4093-31-6 as follows. 4093-31-6

Stage B Preparation of 4-amino-5-chloro-2-methoxybenzoic acid Methyl 4-acetamido-5-chloro-2-methoxybenzoate is dissolved in ethanol and aqueous potassium hydroxide added. The solution is refluxed for a short time, cooled and concentrated hydrochloric acid added. The resulting precipitate is filtered off, washed with water and dried to give the title compound as a white solid.

According to the analysis of related databases, 4093-31-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Palmer, Richard Michael John; Meyers, Nicholas Leslie; Knight, John; US2005/49416; (2005); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics