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1,5,6-Oxadithionane-2,9-dione synthesis

2synthesis methods
-

Yield:24057-56-5 73%

Reaction Conditions:

with acetyl chloride for 5 h;Reflux;

Steps:

4 Example 4: Synthesis of camptothecin dithiodipropionate

Dithiodipropionic acid (2 g, 9.51 mmol) was dissolved in acetyl chloride (15 mL) and refluxed for 5 hours. Then remove the solvent With agents, the filter residue is precipitated in excess ice ether and dried to obtain the crude product of dithiodipropionic anhydride. Add to a 100mL round bottom flaskAdd the prepared dithiodipropionic anhydride (1.24g, 6.45mmol) and camptothecin (0.45g, 1.29mmol), and then dissolve it with pyridine,Under nitrogen protection, stirring under ice bath, pyridine solution of DMAP (0.16g, 1.29mmol) was added to the system. Then mix the solutionHeat to 70°C and continue to react for 48h in an ice bath. The reaction solution was extracted with chloroform and dilute hydrochloric acid, and dried in vacuum to obtain dithio0.51g camptothecin dipropionate, with a yield of 73%.

References:

CN111358948,2020,A Location in patent:Paragraph 0052-0053