According to the analysis of related databases, 63624-28-2, the application of this compound in the production field has become more and more popular.
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 63624-28-2 as follows. Application In Synthesis of 2,4-Dimethoxybenzene-1-sulfonyl chloride
620 mg of the compound obtained in step 15-1 (diastereoisomer mixture) was added under ice cooling and a nitrogen atmosphere to a 10 mL N,N-dimethylformamide solution of 67 mg of sodium hydride, and the reaction mixture was stirred for 40 minutes. After this, a 2 mL N,N-dimethylformamide solution of 400 mg of 2,4-dimethoxybenzenesulfonyl chloride was added dropwise. The reaction mixture was stirred for 30 minutes at the same temperature, after which 5 mL of ethyl acetate and 10 mL of a 5% potassium carbonate aqueous solution were added, and the reaction mixture was stirred at room temperature overnight. The precipitated solids were filtered off and separated and purified by column chromatography (silica gel 60, mobile phase: ethyl acetate/acetone = 99/1; v/v) to obtain two kinds of diastereoisomer of the titled compound in amounts of 184 mg (isomer A: colorless, amorphous) and 256 mg (isomer B: colorless, amorphous). Isomer A: [alpha]D25 = -225 (c = 0.187, chloroform) MS (ESI pos.) m/z : 612([M+H]+), (ESI pos.) m/z : 634([M+Na]+) 1 H-NMR (499 MHz, CDCl3) delta (ppm) ; 1.53 – 1.62 (m, 1 H), 1.85-1.98 (m, 1 H), 2.18 – 2.32 (m, 7 H), 2.75 (s, 3 H), 3.10-3.25 (m, 1 H), 3.55-3.86 (m, 9 H), 4.89-5.01 (br, 1 H), 5.21 – 5.39 (m, 1 H), 6.40 (d, J=1.8 Hz, 1 H), 6.58 (dd, J=9.0, 2.3 Hz, 1 H), 6.76 (d, J=7.9 Hz, 1 H), 6.85 – 6.97 (m, 2 H), 7.07 (dd, J=8.5, 1.2 Hz, 1 H), 7.17 – 7.24 (m, 1 H), 7.74 – 7.84 (m, 2 H), 8.15 (d, J=8.8 Hz, 1 H) Isomer B: [alpha]D25 =+142 (c = 0.240, chloroform) MS (ESI pos.) m/z : 612([M+H]+), (ESI pos.) m/z : 634([M+Na]+) 1 H-NMR (499 MHz, CDCl3) delta (ppm) ; 1.81 – 1.96 (m, 1 H), 2.11 – 2.23 (m, 4 H), 2.46 (s, 3 H), 2.62 (s, 3 H), 3.24 (s, 3 H), 3.36 – 3.49 (m, 1 H), 3.73 – 3.87 (m, 7 H), 4.06-4.11 (m, 1 H), 5.00 – 5.15 (m, 1 H), 6.47 (d, J=2.4 Hz, 1 H), 6.60 (dd, J=9.0, 2.3 Hz, 1 H), 6.66 – 6.73 (m, 2 H), 7.03 – 7.10 (m, 2 H), 7.18 – 7.24 (m, 1 H), 7.81 (d, J=8.2 Hz, 1 H), 8.15-8.25 (m, 2 H)
According to the analysis of related databases, 63624-28-2, the application of this compound in the production field has become more and more popular.
Reference:
Patent; TAISHO PHARMACEUTICAL CO., LTD; EP1659121; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics