Gamma-aminobutyric acid derivative and its preparing process
A technology of aminobutyric acid and derivatives, applied in the field of γ-aminobutyric acid derivatives, can solve problems such as increasing drug stability
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Embodiment 1
[0022] Example 1 Compound I 1 preparation of
[0023] Add 8gNaOH and 150ml water into the reaction flask, stir to dissolve, cool in an ice bath, add 31.8g of pregabalin, and drop 52.4g of BOC anhydride-250ml dioxane solution and 8.8gNaOH-220ml aqueous solution at the same time after completely dissolving. The rate of addition is such that the pH of the reaction solution is controlled at about 9, and the addition is completed in about 1 hour. Then continue to react for 2h, rise to room temperature for 2h. Stop the reaction, extract excess BOC anhydride in the reaction solution with ether, extract 4 times, consume 250ml of ether each time, discard. Adjust the pH of the water phase to about 3 with 5% citric acid solution, extract 3 times with ethyl acetate, 600ml each time, combine the organic phases, wash 3 times with water, wash 3 times with saturated brine, and dry over anhydrous magnesium sulfate for more than 4 hours. After filtration and concentration, 44.5 g of BOC-preg...
Embodiment 2
[0026] Example 2 Compound I 2 preparation of
[0027] Referring to the method of Example 1, BOC-D-serine was replaced by BOC-L-serine to obtain compound I 2 . Elemental Analysis C 11 h 24 N 2 o 4 Cl 2 : Calculated (, %): C 41.38, H 7.52, N 8.78; Measured (, %): C 41.62, H 7.54, N 8.56. MS (ESI, m / e): 247.1 (M+1).
Embodiment 3
[0028] Example 3 Compound I 3 preparation of
[0029] Referring to the method of Example 1, BOC-L-threonine was replaced by BOC-L-serine to obtain compound I 3 . Elemental Analysis C 12 h 26 N 2 o 4 Cl 2 : Calculated value (, %): C 43.24, H 7.81, N 8.41; Measured value (, %): C 43.02, H 7.70, N 8.38. MS (ESI, m / e): 260.9 (M+1).
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