* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With dihydrogen peroxide In water at 20℃; for 12 h;
) Pure MCS (0.2 mol) obtained in step (2) was dissolved in 300 mL of distilled water, and 0.25 mol of hydrogen peroxide solution (30percent) was slowly added with magnetic stirring, and stirring was continued at room temperature for 12 h to obtain a crude MCSO solution. The insoluble impurities in the solution were removed by filtration, and then 2 L of absolute ethanol was added and after placing it at 4 ° C for 12 h the MCSO crystals were formed. The crystals were filtered and dried at 50 ° C to give 28 g of MCSO. [0049] (4) The MCS0 crystal obtained in step (3) was dissolved in 120 mL of distilled water, heated to 50 ° C, added to a 50 ° C first dilute acetone solution (77 mL of distilled water + 394 mL of acetone) and cooled to room temperature. The solution was allowed to stand at 4 ° C for 6-12 hours for crystallization. After drying , 6.9 g of crystals were filtered, redissolved in 23 mL of distilled water, 50 ° C of a second dilute acetone solution (19 mL of distilled water + 95 mL of acetone) was added, the mixture was filtered hot, cooled to room temperature, and the solution was placed at 4 ° C for 6- 12h for crystallization. After filtration and drying , the obtained 3.5 g of crystals was redissolved in 11.5 mL of distilled water, a 50 ° C solution of the third dilute acetone (10 mL of distilled water + 45 mL of acetone) was added, the mixture was filtered hot, cooled to room temperature, and the solution was placed at 4 ° C -12h for crystallization,to obtain a pure (+) MCSO of about 2.82g. [0050] Take the amount of MCSO sample dried to constant weight, accurately weighed, dissolved in distilled water to make 1mg / mL solution, 20 ° C, the wavelength of 589.3nm, using 10mm microtube in the WXG-4 disk polarimeter detection.
Reference：
[1] Journal of agricultural and food chemistry, 2002, vol. 50, # 16, p. 4445 - 4451
[2] Biochimie, 2016, vol. 128-129, p. 92 - 98
[3] Tetrahedron, 1998, vol. 54, # 5-6, p. 735 - 742
[4] Journal of the American Chemical Society, 1999, vol. 121, # 24, p. 5799 - 5800
[5] Journal of Agricultural and Food Chemistry, 2000, vol. 48, # 11, p. 5731 - 5735
[6] Journal of Agricultural and Food Chemistry, 2000, vol. 48, # 12, p. 6254 - 6260
[7] Patent: WO2014/9759, 2014, A2, . Location in patent: Page/Page column 75
[8] Patent: WO2015/8019, 2015, A1, . Location in patent: Page/Page column 84
[9] Patent: CN104140384, 2016, B, . Location in patent: Paragraph 0048; 0049
2
[ 1187-84-4 ]
[ 3226-62-8 ]
[ 6853-87-8 ]
Reference：
[1] Journal of the American Chemical Society, 1956, vol. 78, p. 1605,1606
[2] Zeitschrift fuer Naturforschung, 1957, vol. 12b, p. 687,695
[3] Biochemical Journal, 1956, vol. 64, p. 252,257
[4] Pr.roy.Soc.<B>, 1951, vol. 138, p. 265,270
With dihydrogen peroxide; In water; at 25℃; for 24h;
2. Preparation of Methiin (P-i: S-methvl-L-cysteine suiphoxide):S-Methyl-L-cysteine (5g - obtained from Dickrna) was dissolved in 25 ml water and whilst the solution was stirred 5.5 ml of 30% rn/rn hydrogen peroxide was added dropwise whilst the solution temperature was maintained at 25 C. The solution wasstirred for 24 hours during which time the temperature was maintained at 25 C. After this period, the solvent was removed at 60C under vacuum using a rotary evaporator. The white residue was dissolved in the minimum volume of acetone:water:acetic acid (65:34:1 v/v) whose temperature was 45 C with methiin crystals forming on cooling at 4 C. The methiin crystals were isolated by filtration and were washed with two 25ml aliquots of cold acetone. Thereafter, the rnethiin was air dried at 25 C and then stored at 4 C prior to use.
With dihydrogen peroxide; In water; at 25℃; for 24h;
S-Methyl-L-cysteine (5g - obtained from Dickma) was dissolved in 25 ml water and whilst the solution was stirred 5.5 ml of 30% m/m hydrogen peroxide was added dropwise whilst the solution temperature was maintained at 25 C. The solution was stirred for 24 hours during which time the temperature was maintained at 25 C. After this period, the solvent was removed at 60 C under vacuum using a rotary evaporator. The white residue was dissolved in the minimum volume of acetone:water:acetic acid (65:34: 1 v/v) whose temperature was 45 C with methiin crystals forming on cooling at 4 C. The methiin crystals were isolated by filtration and were washed with two 25 ml aliquots of cold acetone. Thereafter, the methiin was air dried at 25 C and then stored at 4 C prior to use.
2.82 g
With dihydrogen peroxide; In water; at 20℃; for 12h;
) Pure MCS (0.2 mol) obtained in step (2) was dissolved in 300 mL of distilled water, and 0.25 mol of hydrogen peroxide solution (30%) was slowly added with magnetic stirring, and stirring was continued at room temperature for 12 h to obtain a crude MCSO solution. The insoluble impurities in the solution were removed by filtration, and then 2 L of absolute ethanol was added and after placing it at 4 C for 12 h the MCSO crystals were formed. The crystals were filtered and dried at 50 C to give 28 g of MCSO. [0049] (4) The MCS0 crystal obtained in step (3) was dissolved in 120 mL of distilled water, heated to 50 C, added to a 50 C first dilute acetone solution (77 mL of distilled water + 394 mL of acetone) and cooled to room temperature. The solution was allowed to stand at 4 C for 6-12 hours for crystallization. After drying , 6.9 g of crystals were filtered, redissolved in 23 mL of distilled water, 50 C of a second dilute acetone solution (19 mL of distilled water + 95 mL of acetone) was added, the mixture was filtered hot, cooled to room temperature, and the solution was placed at 4 C for 6- 12h for crystallization. After filtration and drying , the obtained 3.5 g of crystals was redissolved in 11.5 mL of distilled water, a 50 C solution of the third dilute acetone (10 mL of distilled water + 45 mL of acetone) was added, the mixture was filtered hot, cooled to room temperature, and the solution was placed at 4 C -12h for crystallization,to obtain a pure (+) MCSO of about 2.82g. [0050] Take the amount of MCSO sample dried to constant weight, accurately weighed, dissolved in distilled water to make 1mg / mL solution, 20 C, the wavelength of 589.3nm, using 10mm microtube in the WXG-4 disk polarimeter detection.
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