Synthesis
The sublimation reaction was carried out at 220 °C and under vacuum conditions (~10 mbar) using 4-hydroxyphthalic acid (1 g, 5.49 mmol) as the raw material. Upon completion of the reaction, the resulting white solid 5-hydroxyisobenzofuran-1,3-dione (675 mg, 4.11 mmol, 74.9% yield, MS/ESI+ 164.9 [MH]+) was collected. The product is to be stored under vacuum and used directly in subsequent reaction steps.
References
[1] Bioorganic and Medicinal Chemistry Letters, 2005, vol. 15, # 20, p. 4427 - 4431
[2] Journal of Medicinal Chemistry, 2011, vol. 54, # 1, p. 342 - 353
[3] Patent: CN104910113, 2017, B. Location in patent: Page/Page column 0041; 0044-0046
[4] European Journal of Medicinal Chemistry, 1987, vol. 22, p. 229 - 238
[5] Patent: US2013/102576, 2013, A1. Location in patent: Paragraph 0607