A substantial quantity of 2-phenol-benzothiazole must be synthesized. Benzothiazole (1 mmol), 2-hydroxyiodobenzene (1 mmol), and K2CO3 (2 mmol) as a binding agent were combined in 2 mL of DMSO. The resulting mixture is magnetically stirred at 120°C for 6 h, with the reaction progress monitored via TLC. Upon completion, the reaction mixture was cooled to room temperature, and the solvent is evaporated under reduced pressure. Following this, water (8 mL) and an equivalent volume of ethyl acetate were introduced for extraction through multiple iterations of small-volume extractions (3 times). The aqueous layer was discarded, and the organic layer was desiccated with Na2SO4. Subsequent to drying, the organic layer underwent evaporation under reduced pressure, and the resulting residue was subjected to column chromatography. Intermediate 1 was extracted through column chromatography using a mobile phase of petroleum ether: ethyl acetate = 2:1. The yield is 50%, and the product was dried in an oven for subsequent use.
Free full text: Click here