Rapid and safe preparation method of triptolide triol

[0037] Example 1

[0038]

[0039] Weigh about 0.8 g of sodium dihydrogen phosphate, add 500 mL of ultrapure water to dissolve, add a volume fraction of 1% phosphoric acid solution to adjust the pH to 4.0 at room temperature, and obtain a phosphate buffer solution with a pH of 4.

[0040] Take 0.5 g of triptolide and place it in a 20 mL microwave reaction flask, add 10 mL of the prepared phosphate buffer solution to dissolve and seal. Make it mix well, set 140℃ to react for 1.5h. After the reaction, the reaction liquid was a yellow solution. The mother liquor of the compound represented by formula (I) is obtained.

[0041] Put the yellow solution after the reaction on a rotary evaporator and quickly drain the solvent. The remaining solids are reconstituted with methanol. The pipette will extract the reconstituted product into a centrifuge tube. After high-speed centrifugation, the pipette will extract the supernatant to the front end for fixation. A syringe tube with a 0.22μm filter

[0067] Example 2

[0068]

[0069] The microwave heating conditions were set to 155°C, the reaction time was 40 minutes, the phosphate buffer solution was adjusted to pH=3.5, and the rest of the operation was the same as in Example 1. Finally, 266.8 mg of triptolide was obtained, and the yield was 50.82%. The purity is 98.3%, and the rest of the structure test data is the same as in Example 1.

[0070] Example 3

[0071]

[0072] Weigh NaH 2 PO 4 ·H 2 O 27.6g, add heavy distilled water to 1000mL to dissolve. Configure into a liquid nail. Weigh Na 2 HPO 4 ·2H 2 O 35.6g add heavy distilled water to 1000mL to dissolve, prepare into B liquid. Take 5.3 mL of A solution and 94.7 mL of B solution and mix to obtain a phosphate buffer with pH=8.0.

[0073] Take 0.5 g of triptolide and place it in a 20 mL microwave reaction flask, add 10 mL of the prepared phosphate buffer solution with pH=8.0 to dissolve and seal. Mix well and set 160°C to react for 25 minutes. After the reaction, the reaction liquid was a yellow solution. The mother liquor of the compound represented by formula (I) is obtained.

[0074] The yellow solution after the reaction was frozen, and the solvent was drained by a freeze dryer to obtain a yellow powder. The remaining operations are the same as in Example 1. Obtained 282.3g of triptolide triol with a yield of 53.77%. The rest of the structure test data is t