2-hydroxyhexahydro-1H-isoindole-1,3(2H)-dione synthesis

Yield:18886-85-6 94%

Reaction Conditions:

with hydroxyammonium sulfate;sodium hydroxide in water at 90; for 1.25 h;

Steps:

22 Reference Example 22(3aR, 7aS) -2- hydroxy-hexahydro -1H- isoindole -1,3 (2H) - dione

hydroxylamine sulfate (24.975g, 0.152mol) was dissolved in water (75mL) was added (3aR, 7aS) - hexahydro-isobenzofuran-1,3-dione (48.000g). Takes 15 minutes to the mixture little by little added 25% aqueous sodium hydroxide (50g), was stirred at 90 1 hour. The mixture was cooled to room temperature and extracted twice with 50mL of chloroform, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under reduced pressure, the residue was dissolved in chloroform, insoluble matter was filtered, the solvent was concentrated under reduced pressure. Ethyl acetate was added to dissolve the residue, the solvent was concentrated under reduced pressure, and further dried in vacuo 2, to give the title compound as a colorless solid, 49.35g (94% yield).

References:

CN105555787,2016,A Location in patent:Paragraph 0561; 0562; 0563; 0564; 0565; 0566