Category: 7700-07-4

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. 7700-07-4, name is N,N-Dimethylethenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of N,N-Dimethylethenesulfonamide

General procedure: A dried 25 ml, screw-sealed tube was charged with degassed [1,4 dioxane/water, 3 ml, 99:1 (v/v)], followed by the addition of 6 (140 mg, 1 mmol) and 3-chlorophenylboronic acid (624 mg, 4 mmol). After addition of [RhOH(cod)]2 (2 mol %, 9.1 mg, 0.02 mol) and rac-BINAP (6 mol %, 37 mg, 0.06 mol), the tube was closed. After removing air by vacuum the tube was back-filled with nitrogen and heated in a pre-heated oil bath at 120 C for 18 h. After cooling to room temperature, the resulting mixture was diluted with EtOAc (5 ml) and extracted with 5% aqueous NaHCO3 solution (5 ml). The organic layer was dried over Na2SO4 and concentrated in vacuo. The crude obtained 7 was further purified by flash chromatography [silica gel 60 (0.040-0.063 nm, Merck)] eluent, Et2O-petroleum ether (40-60), 3:1 (v/v) or CH2Cl2 – EtOAc,, 95:5 (v/v), to give 158 mg of pure 7 (64%).

The synthetic route of 7700-07-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zilaout, Hicham; Van Den Hoogenband, Adri; De Vries, Jelle; Lange, Jos H.M.; Terpstra, Jan Willem; Tetrahedron Letters; vol. 52; 45; (2011); p. 5934 – 5939;,
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. 7700-07-4, name is N,N-Dimethylethenesulfonamide, A new synthetic method of this compound is introduced below., COA of Formula: C4H9NO2S

(i) 2-(1H-Indol-5-yl)-N,N-dimethylethenesulphonamide A mixture of 5-bromoindole (7.7 g), N,N-dimethylethenesulphonamide (5.3 g) triethylamine (15 ml), acetonitrile (5 ml), palladium (II) acetate (0.35 g) and tri-o-tolylphosphine (0.95 g) was heated at 100 C. in an autoclave for 3 h. The resulting cooled mixture was partitioned between hydrochloric acid (2N, 300 ml) and ethyl acetate (2*150 ml). The combined extracts were dried (Na2 SO4) and evaporated in vacuo. The residue was purified by `flash` chromatography (V, 7 cm col.) to give the title compound as a crystalline solid (3.8 g) m.p. 148-150 C.

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; Glaxo Group Limited; US4994483; (1991); A;,
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. 7700-07-4, name is N,N-Dimethylethenesulfonamide, A new synthetic method of this compound is introduced below., COA of Formula: C4H9NO2S

To a solution of Example 1.18.18 (69.8 mg) in N,N-dimethylformamide (6 mL) was added N,N-dimethylethenesulfonamide (118 mg), N,N-diisopropylethylamine (0.2 mL) and H20 (0.2 mL). The mixture was stirred at room temperature 4 days. The reaction mixture was diluted with ethyl acetate (200 mL), washed with water and brine, and dried over anhydrous sodium sulfate. After evaporation of the solvent, the residue was dissolved in dichloromethane and trifluoroacetic acid (10 mL, 1 :1), and the resulting solution was stirred overnight. The solvents were removed under reduced pressure. The residue was diluted with N,N-dimethylformamide (2 mL), filtered and purified by reverse-phase HPLC on a Gilson system (CI 8 column), eluting with 20-80% acetonitrile in water containing 0.1% trifluoroacetic acid, to give the title compound. NMR (400 MHz, dimethyl sulfoxide-^) delta ppm 12.82 (s, 1H), 8.53 (s, 2H), 8.00 (dd, 1H), 7.76 (d, 1H), 7.59 (dd, 1H), 7.53 – 7.37 (m, 4H), 7.37 – 7.28 (m, 2H), 7.26 (s, 1H), 6.92 (d, 1H), 4.92 (s, 2H), 3.80 (s, 2H), 3.54 (t, 2H), 3.44 – 3.34 (m, 2H), 3.30 (s, 2H), 3.11 (s, 2H), 2.98 (t, 2H), 2.77 (s, 6H), 2.07 (s, 3H), 1.39 (s, 2H), 1.27 (q, 4H), 1.11 (s, 4H), 1.06 – 0.93 (m, 2H), 0.83 (s, 7H). MS (ESI) m/e 881.2 (M+H)+.

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; ABBVIE INC.; BENATUIL, Lorenzo; BRUNCKO, Milan; JUDD, Andrew, S.; LI, Yingchun; MCCLUSKEY, Andrew; PHILLIPS, Andrew, C.; PHILLIPS, Darren, C.; SEAGAL, Jane; SOUERS, Andrew, J.; (608 pag.)WO2017/214458; (2017); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics