a
Department of Chemistry, Xi‘an-Jiaotong Liverpool University, Suzhou, Jiangsu Province, 215123, P. R. of China
b
Department of Chemistry, University of Liverpool, Liverpool, L69 7ZD, UK
› InstitutsangabenThis work was supported by the Research Development Fund (RDF-20-02-30), PGRS2112027, and FOSA2212021) from Xi’an Jiaotong-Liverpool University.
Herein, we present a rapid and efficient method for synthesizing cyclic acetals and ketals utilizing a rotary evaporator. Unlike the conventional Dean–Stark dehydration process, which typically demands extended reaction times and copious amounts of organic solvents, our approach affords the synthesis of cyclic acetals and ketals with varying ring sizes in 30 min while using minimal quantities of dimethyl sulfoxide as the solvent. This innovative protocol features high yields, fast reactions, easy operation, and broad substrate applicability.
17General Procedure for Synthesizing Dioxalanes
The temperature of the coolant-circulation system was fixed at 0 ℃, and the rotation speed was set to 100 rpm. To a round-bottom flask, aldehyde (10 mmol), diol (30 mmol), and the corresponding acid (1 mmol) were dissolved in 0.5–2 mL DMSO, which was heated on a rotavap at 30 mbar for 0.5 h. The product is purified by silica gel chromatography.
18General Procedure for Synthesizing Dioxanes
The temperature of the coolant-circulation system was fixed at 0 ℃, and the rotation speed was set to 100 rpm. To a round-bottom flask, aldehyde/ketone (10 mmol), diol (20 mmol), and the corresponding acid (1 mmol) were dissolved in 0.5–2 mL DMSO, which was heated on a rotavap at 30 mbar for 0.5 h. The product is purified by silica gel chromatography.
