Tiopronin amidate and its prepn
A technology of tiopronin amino acid salt and amino acid, which can be applied in pharmaceutical formulations, medical preparations containing active ingredients, digestive system, etc. And other issues
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Embodiment 1
[0029] Embodiment 1: the preparation of tiopronin arginine salt
[0030] raw material name
Feeding amount
Tiopronin
L-Arginine
Methanol (95%)
100g
112g
600ml
1
1.05
[0031] operate:
[0032] Put tiopronin, L-arginine, and methanol into a 1000ml three-neck reaction flask, stir, heat to reflux, and after 3 hours of reflux reaction, filter while hot, and place the filtrate in a refrigerator at 5-10°C to cool and crystallize. After 5 hours, it was filtered to obtain white crystals, which were dried in an oven at 80°C for 6 hours to obtain 196 g of white crystalline solids, yield 94.8%, mp 197-200°C.
[0033] The infrared absorption spectrum data of the sample:
[0034] Absorption peak (cm -1 ): 2957.92, 1647.58, 1604.88, 1525.77, 1457.23, 1407.90, 1386.21, 1357.38, 1335.77, 1313.99, 1246.37, 1159.37, 1012.96, 670.43, 555.97.
Embodiment 2
[0035] Embodiment 2: the preparation of tiopronin lysine salt
[0036] raw material name
Feeding amount
Tiopronin
L-Lysine
Ethanol (95%)
100g
94g
600ml
1
1.0
[0037] operate:
[0038] Put tiopronin, L-lysine, and ethanol into a 1000ml three-necked reaction flask, stir, heat to reflux, and after 3 hours of reflux reaction, filter while hot, and place the filtrate in a refrigerator at 5-10°C to cool and crystallize. After 5 hours, it was filtered to obtain white crystals, which were dried in an oven at 80° C. for 6 hours to obtain 177 g of white crystalline solids, yield 93.4%, mp 172-175° C.
[0039] The infrared absorption spectrum data of the sample:
[0040] Absorption peak (cm -1 ): 3328.57, 2939.20, 1646.85, 1593.90, 1521.17, 1405.00, 1357.70, 1316.94, 1023.31, 904.87, 701.58, 550.03, 420.12.
Embodiment 3
[0041] Embodiment 3: the preparation of tiopronin ornithine salt
[0042] raw material name
Feeding amount
Tiopronin
90% aqueous methanol
100g
89g
500ml
1
1.1
[0043] operate:
[0044] Put 100g of tiopronin, 89g of ornithine, and 500ml of 90% aqueous methanol into a 1000ml three-neck reaction flask, stir, heat to reflux, and after 3 hours of reflux reaction, filter while hot, and put the filtrate in a refrigerator at 5-10°C to cool and crystallize. After 5 hours, it was filtered to obtain white crystals, which were dried in an oven at 80°C for 6 hours to obtain white crystalline solids, mp 238-240°C.
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