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L-alliin was obtained from the amino acid L-deoxyalliin by an oxidative process with hydrogen peroxide in a procedure similar to that described in the literature [18,19]. Anal. Calcd for C6H11NO3S × 0.5 H2O (%): C 38.7 H 6.51 N 7.52. Found (%): C 38.1 H 6.29 N 7.49.
With dihydrogen peroxide; In water; at 25℃; for 24h;
L-Deoxyalliin (5g - as prepared in step (i) above) 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 alliin crystals forming on cooling at 4 C. The alliin crystals were isolated by filtration and were washed with two 25 ml aliquots of cold acetone. Thereafter, the alliin was air dried at 25 C and then stored at 4 C prior to use.
3.3 g
With dihydrogen peroxide; In water; at 20℃; for 12h;
Pure 2-PeCS (0.2 mol) obtained in step (2) was dissolved in 250 mL of distilled water, 0.28 mol of a hydrogen peroxide solution (30%) was slowly added with magnetic stirring, and stirring was continued at room temperature for 12 h to obtain crude 2- PeCSO solution.The insoluble impurities in the solution were removed by filtration, and then 2 L of anhydrous ethanol was added and 6 C was placed at 4 C to form 2-PeCSO crystals.The crystals were filtered to dry at 40 C to give 33.6 g of thioallyl cysteine sulfoxide (2-PeCSO).(4) The 2-PeCSO crystal obtained in step (3) was dissolved in 150 mL of distilled water, heated to 50 C, and a first dilute acetone solution (96 mL of distilled water + 492 mL of acetone) at 50 C was added and cooled to room temperature.The solution was allowed to stand at 4 C for 12 h.(8.2.4 mL of distilled water + 112 mL of acetone) was added at 50 C, the mixture was filtered hot, cooled to room temperature, and the solution was allowed to stand at 4 C for 12 hours to crystallize.(11 mL of distilled water + 50 mL of acetone) at 50 C, and the mixture was filtered through hot, cooled to room temperature, and the solution was allowed to stand at 4 C for 12 hours to give pure crystals. The solution was purified by filtration and dried in 15 mL of distilled water. (+) 2-PeCSO about 3.3g.
With dihydrogen peroxide; at 20℃;
ACSO synthesis was performed as previously describedwith some modifications [13,14]. l-Cysteine methyl esterhydrochloride (3.0 g, 5.83 mmol) was dissolved in ethanol/H2O (2:1, v/v, 30 mL), before triethylamine (7.2 mL,17.2 mmol) and allyl bromide (2.9 mL, 10.4 mmol) wereadded. After stirring for 20 min, the reaction mixturewas then filtered and concentrated in vacuo to yieldS-allyl-L-cysteine (white crystals). S-allyl-L-cysteine wasdissolved in water and the 30% w/w hydrogen peroxide(weight of S-allyl-L-cysteine (g) × 1.26 mL) was added.After stirring overnight at room temperature, the solutionwas filtered in vacuo. Then, the filtrate was mixedwith 1% acetate (5 mL) and 99.5% ethanol (75 mL) at160 C. The reaction mixture was cooled to 4 C andstirred for 60 min and then all solvents and reagentswere removed in vacuo. Without further procedures,the ACSO (white crystals) obtained should have been of sufficient purity for use in animal experiments andthis was confirmed from NMR spectra recorded on anECA500 spectrometer (JEOL, Tokyo, Japan).
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