Category: 326-67-0

Reference of 326-67-0,Some common heterocyclic compound, 326-67-0, name is N-(2-Fluoro-4-methylphenyl)acetamide, molecular formula is C9H10FNO, 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.

To 546 g (3.27 mol) of crude 2-fluoro-4-methyl-acetanilide was added chlorosul- phonic acid (2000 g, 17.24 mol) with stirring at a temperature below 70C. Stirring was continued for 3 hours at a temperature of 70C. The reaction mixture was poured onto ice and then extracted with ethyl acetate. The organic phase was dried with sodium sulfate and concentrated under reduced pressure to yield the title compound (500 g, 57.8%). H NMR (400 MHz, CDCI3): delta = 9.1 (d, 1 H, J = 7.2 Hz), 7.39-7.52 (m, 1 H), 7.14 (d, 1 H, J = 1 1 .2 Hz), 2.72-2.78 (m, 3H), 2.2-2.3 (m, 3H).

The synthetic route of 326-67-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BASF SE; KAISER, Florian; GROss, Steffen; LANGEWALD, Juergen; NARINE, Arun; WO2013/30262; (2013); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 326-67-0, 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 326-67-0 as follows.

Chlorosulfonic acid (20.56 g, 176.46 mmol, 5 equiv.) was slowly added to N-(2-fluoro-4-methylphenyl) acetamide (5.90 g,35.29 mmol, 1 equiv.) keeping the temperature of the reactionmixture below 50 C. The resulting mixture was then heated to70 C for 4 hours. After cooling to room temperature, thereaction mixture was then poured carefully into ice, the precipitate was filtered, washed well with distilled water and dried to get 7.3 g of crude product as light brown solid. The crude product thus obtained was further used as such without any purification.?H NMR (CDC13) : 6 9.09 (d, J = 7.6 Hz, 1H), 7.48 (bs, 1H), 7.14 (d, J = 10.8 Hz, 1H) , 2.72 (s, 3H) , 2.25 (s, 3H)

According to the analysis of related databases, 326-67-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; INSECTICIDES (INDIA) LIMITED; OAT AGRIO CO., LTD; IMAI, Tetsuya; KUMAWAT, Surendra Kumar; SINGH, Manish Kumar; CHAUHAN, Pramod Kumar; SHELKE, Amol Vasant; SINGH, Rajesh Kumar; KISHORE, Ram; BHATT, Ashish; (97 pag.)WO2018/15852; (2018); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 326-67-0, name is N-(2-Fluoro-4-methylphenyl)acetamide, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H10FNO

A solution of the acetamide from preparation 26 (1.0 g, 5.9 mmol) in nitric acid (70%, 10 ml) was cooled to 0 C. and treated with fuming nitric acid (90%, 10 ml) maintaining the reaction temperature <0 C. The reaction was left to stir for one hour at 0 C. and then poured onto ice and allowed to warm gradually to room temperature. The resulting precipitate was collected by filtration and dried in vacuo to give a colourless solid (1 g, mixture of isomers). The solid was dissolved in methanol (20 ml) and solid KOH added to adjust the pH to 10. The solution was left to stir at room temperature for 16 hours and then the solvent was removed in vacuo. Water (50 ml) and dichloromethane (50 ml) were added and the organic phase separated. The aqueous phase was extracted with further dichloromethane (50 ml) and the combined organics dried (sodium sulphate) and reduced in vacuo. Purification by flash column chromatography on silica gel eluting with pentane:ethyl acetate (80:20 changing to 20:80, by volume) gave the title compound as a yellow solid (124 mg). 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; Lane, Charlotte Alice Louise; Price, David Anthony; US2006/111416; (2006); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

326-67-0, A common heterocyclic compound, 326-67-0, name is N-(2-Fluoro-4-methylphenyl)acetamide, molecular formula is C9H10FNO, its 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.

Chlorosulfonic acid(20.56 g,176.46 mmol,5 equiv.)was slowly added to N-(2-fluoro-4-methylphenyl)acetamide(5.90 g,35.29 mmol,1 equiv.)keeping the temperature of the reaction mixture below 50 C. The resulting mixture was then heated to 70 C for 4 hours. After cooling to room temperature,the reaction mixture was then poured carefully into ice,the precipitate was filtered,washed well with distilled water and dried to get 7.3 g of crude product as light brown solid. The crude product thus obtained was further used as such without any purification. NMR(CDCI3): delta 9.09(d,J = 7.6 Hz,1H),7.48(bs,1H),7.14(d, J = 10.8 Hz,1H),2.72(s,3H),2.25(s,3H).

The synthetic route of N-(2-Fluoro-4-methylphenyl)acetamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; INSECTICIDES (INDIA) LIMITED; OAT AGRIO CO., LTD.; IMAI, Tetsuya; KUMAWAT, Surendra Kumar; SINGH, Manish Kumar; CHAUHAN, Pramod Kumar; BHATT, Ashish; SURAMWAR, Nikhil Vilas; SHELKE, Amol Vasant; SINGH, Rajesh Kumar; KISHORE, Ram; (138 pag.)WO2018/51252; (2018); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics