Category: 22503-72-6

Synthetic Route of 22503-72-6, These common heterocyclic compound, 22503-72-6, name is 7-Chloro-3-methyl-3,4-dihydro-2H-benzo[e][1,2,4]thiadiazine 1,1-dioxide, 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.

General procedure: To an ice-cooled solution of 2,3-dihydrobenzothiadiazine 1 or 6-13(1.0 mmol) in CH2Cl2 (10 mL) was added dropwise an excess ofMCPBA (739 mg, 3.0 mmol, 70%) in CH2Cl2 (10 mL) previouslycooled in an ice bath. The mixture was allowed to gradually warmto r.t., with stirring, over 12 h. TLC and LC-MS analyses were usedto monitor reaction progress. The solution was then evaporated todryness, in vacuo at r.t., to give the crude material. The reactionmixture was purified by chromatography on silica gel (petroleumether-EtOAc, 60:40).

The synthetic route of 22503-72-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Cannazza, Giuseppe; Perrone, Serena; Rosato, Francesca; D’Accolti, Lucia; Parenti, Carlo; Troisi, Luigino; Synthesis; vol. 46; 7; (2014); p. 962 – 966;,
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 22503-72-6 as follows. Product Details of 22503-72-6

To an ice-cooled solution of 1 (233 mg, 1.0 mmol) in CH2Cl2 (10mL) was added dropwise an excess of MCPBA (1478 mg, 6.0mmol, 70%) in CH2Cl2 (10 mL) previously cooled in an ice bath.The mixture was allowed to gradually warm to r.t., with stirring,over 12 h. TLC and LC-MS analyses were used to monitor reactionprogress. When the reaction was complete, the solution was stirredwith excess powered anhydrous Na2CO3 until carbon dioxide evolutionceased. After filtration, the mixture was concentrated in vacuoat r.t. to give pure 2.Yield: 275 mg (99%); yellow solid; mp 160-163 C.IR (KBr): 3160, 3101, 2990, 1600, 1550, 1350, 850 cm-1.1H NMR (400.13 MHz, CDCl3): delta = 2.48 (s, 3 H, CH3), 7.63 (d,J = 9.0 Hz, 1 H, ArH), 7.98 (d, J = 9.0 Hz, 1 H, ArH), 8.06 (s, 1 H,ArH), 9.25 (br s, 1 H, NH).13C NMR (100.62 MHz, CDCl3): delta = 16.8, 125.4, 126.9, 133.0,135.8, 138.1, 143.5, 165.7.HRMS (ESI): m/z [M + H]+ calcd for C8H7ClN2O5S: 278.9842;found: 278.9840.

According to the analysis of related databases, 22503-72-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Cannazza, Giuseppe; Perrone, Serena; Rosato, Francesca; D’Accolti, Lucia; Parenti, Carlo; Troisi, Luigino; Synthesis; vol. 46; 7; (2014); p. 962 – 966;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics