s‑acetyl‑l‑glutathione crystals i and ii
A technology of glutathione and crystal, applied in the field of chemistry, can solve the problem that the crystal structure of the compound has not been reported.
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Embodiment 1
[0029] First, S-acetyl-L-glutathione was prepared according to published literature. In this example, S-acetyl-L-glutathione was prepared by using the method described in the patent application of the People's Republic of China with application number 201410310430.3, and the obtained S-acetyl-L-glutathione product was a white solid. Take 10 g of the white solid, place it in 100 ml of a mixture of acetone and water at a volume ratio of 1:1, and heat it to 60° C., the white solid completely dissolves. The reaction system was cooled in an ice-water bath, and crystals were precipitated. After filtration, 9.5 g of crystal product was obtained, and the yield of the crystal was 95%.
Embodiment 2
[0031] Take 10 g of the white solid of S-acetyl-L-glutathione prepared in Example 1, place it in 100 ml of a mixture of ethanol and water with a volume ratio of 1:1, and heat it to 60° C., the white solid is completely dissolved. The reaction system was cooled in an ice-water bath, and crystals were precipitated. After filtration, 9.2 g of crystal product was obtained, and the yield of the crystal was 92%.
[0032] The crystal obtained in embodiment 1 and embodiment 2 carries out X-ray diffraction experiment, finds that both X-ray diffraction Figure 1 Consistently, it was confirmed that the two crystals had the same structure, and they were named as type I crystals of S-acetyl-L-glutathione. figure 1 It is the X-ray diffraction pattern of type I crystal. The X-ray source corresponding to the diffraction pattern is Cu / K-α1, and the incident wavelength λ is 1.54056 angstroms. The X-ray diffraction pattern is represented by 2θ, d and relative intensity greater than 15% (θ is...
Embodiment 3
[0036] Prepare S-acetyl-L-glutathione type I crystal 10g according to the method of embodiment 1 or embodiment 2, place in 10mlH 2 O, heated to 80 ° C, all the I-type crystals dissolved. The reaction system was cooled to room temperature, and 100 ml of anhydrous tetrahydrofuran was added, and crystals were precipitated. After filtration, 7.4 g of crystal product was obtained, and the yield of the crystal was 74%.
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