Green synthesis method of belistat
A technology of belinostat and synthesis method, applied in the field of medicine and chemical industry, can solve problems such as physical health and environmental damage, limited production capacity, long reaction time, etc., and achieve the effects of environmental friendliness, protection safety, and easy operation
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Embodiment 1
[0039] (1) In compound I, R=CH 2 CH 3 As an example, add 51.0g of hydroxylamine hydrochloride, 61.0g of NaOH, and 300mL of purified water into a 1000mL reaction bottle, and react at 25°C for 0.5h to obtain a colorless and transparent solution;
[0040] (2) At 25°C, slowly add 33.1g of compound I to the above reaction solution, the solution changes from colorless to white turbid solution and then quickly to bright yellow clear solution, continue to react for 1h, after the reaction is completed, add 60mL of ethanol, The pH was adjusted to 4.0 with 2 mol / L hydrochloric acid aqueous solution by dropwise addition, a large amount of white solid was precipitated, filtered, washed with purified water, and dried to obtain 29.2 g of off-white solid with a yield of 91.8%.
[0041] HPLC purity: 99.96%.
[0042] HPLC conditions: the mobile phase is water and methanol, gradient elution, the elution program is shown in Table 1.
[0043] Table 1 HPLC elution program
[0044] T(m...
Embodiment 2
[0047] (1) In compound I, R=CH 3 For example, add 51.0g of hydroxylamine hydrochloride, 60.0g of NaOH, and 400mL of purified water into a 1000mL reaction bottle, and react at 10°C for 0.5h to obtain a colorless and transparent solution;
[0048] (2) At 10°C, slowly add 63.5g of compound I to the above reaction solution, the solution changes from colorless to white turbid solution and then quickly to bright yellow clear solution, continue to react for 2h, after the reaction is completed, add 4mol / L The hydrochloric acid aqueous solution was added dropwise to adjust the pH to 5.0, and a large amount of white solid was precipitated, filtered, washed with purified water, and dried to obtain 58.9 g of off-white solid with a yield of 92.5%.
Embodiment 3
[0050] (1) In compound I, R=CH 2 CH 3 For example, add 255.2g of hydroxylamine hydrochloride, 400.0g of NaOH, and 1500mL of purified water into a 3000mL reaction bottle, and react at -5°C for 2 hours to obtain a colorless and transparent solution;
[0051] (2) At -5°C, slowly add 331.4g of compound I to the above reaction solution, the solution changes from colorless to white turbid solution and then quickly becomes a bright yellow clear solution, and the reaction is continued for 6 hours. The pH was adjusted to 3.5 by dropwise addition, a large amount of white solid was precipitated, filtered, washed with purified water, and dried to obtain 297.8 g of off-white solid with a yield of 93.6%.
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