Method for preparing glutathione using hydantoinase
A glutathione and hydantoinase technology, applied in the direction of microorganism-based methods, biochemical equipment and methods, microorganisms, etc., can solve the problems of easy hydrolysis, autorotation peptide, low yield of GSH, high production cost, etc., to achieve Avoid the use of energy ATP, avoid protection and deprotection steps, ensure site-specific effects
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Embodiment 1
[0036] Example 1: Synthesis of 5-carboxyethylhydantoin.
[0037] L-glutamic acid (0.1mol) and potassium cyanate (0.12mol) were dissolved in 50mL of water, with 0.5mol·L -1 Potassium hydroxide solution was used to adjust the pH to 9.0, and the reaction was stirred at 75°C for 2 hours to generate the intermediate product N-carbamoyl L-glutamic acid. Add 0.5mol·L -1 Adjust the pH of the solution to 1-2 with hydrochloric acid, raise the temperature to 100°C and heat to reflux for 0.5 h, cool, filter and dry to obtain a white solid, recrystallize with water, and obtain 13.7 g of white crystal 5-carboxyethylhydantoin, with a yield of 79.5%. m.p.179~181℃; 1 H NMR (DMSO-d 6 , 500MHz) δ: 12.14(s, 1H, COOH), 10.59(s, 1H, NH), 7.91(s, 1H, NH), 4.03~4.00(m, 1H, CH), 2.33~2.30(m, 2H , CH 2 ), 1.95~1.68 (m, 2H, CH 2 ); HRMS(ESI) calcd for C 6 h 8 N 2 NaO 4 [M+Na] + 195.0376, found 195.0374.
Embodiment 2
[0038] Example 2: Synthesis of 5-carboxyethylhydantoin.
[0039] Sodium monohydrogen L-glutamate (0.1mol) and sodium cyanate (0.14mol) were dissolved in 50mL of water, with 0.1mol·L -1 Sodium hydroxide solution was used to adjust the pH to 8.5, and the reaction was stirred at 80°C for 2 hours to generate the intermediate product N-carbamoyl-L-glutamic acid. Add concentrated hydrochloric acid to adjust the pH of the solution to 1-2, raise the temperature to 100°C and heat to reflux for 1.5 hours, cool, filter and dry to obtain a white solid, recrystallize with water to obtain 14.2 g of white crystal 5-carboxyethylhydantoin, the yield is 82.7 % (m.p.179-181°C).
Embodiment 3
[0040] Example 3: Synthesis of N-hydantoyl-S-benzyl-L-cysteine.
[0041] Add 200 mL of DMF to 5-carboxyethylhydantoin (0.1 mol) obtained in Example 1, stir and dissolve at room temperature, add DCC (0.1 mol) and HOBt (0.1 mol), react for 2 hours, filter to remove DCU (dicyclohexyl urea), Take the filtrate. Add S-benzyl-L-cysteine (0.13 mol) and react overnight. Pour into water, add ethyl acetate to extract three times, the extract was dried and then concentrated to obtain a white solid, which was recrystallized from methanol to obtain 33.4 g of white crystal N-hydantoylpropionyl-S-benzyl-L-cysteine , yield 91.4%, m.p.81~83℃; 1 H NMR (DMSO-d 6 , 500MHz) δ: 12.80(s, 1H, COOH), 10.62(s, 1H, NH), 8.25(d, J=8.0Hz, 1H, NH), 7.89(s, 1H, NH), 7.32~7.24( m, 5H, PhH), 4.45~4.41(m, 1H, CH), 4.05~4.03(m, 1H, CH), 3.75(s, 2H, CH 2 ), 2.81~2.63 (m, 2H, CH 2 ), 2.31~2.17 (m, 2H, CH 2 ), 1.96~1.70 (m, 2H, CH 2 ); HRMS(ESI) calcd for C 16 h 19 N 3 NaO 5 S[M+Na] + 388.0938, found...
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