Highly efficient condensation of glycerol to cyclic acetals catalyzed by titanium-exchanged montmorillonite

Heterocycles

Volumn 84, Issue 1, 2011, Pages 371-376

  Mitsudome, Takato ^a   Matsuno, Tsuyoshi ^a   Sueoka, Shoichiro ^a   Mizugaki, Tomoo ^a   Jitsukawa, Koichiro ^a   Kaneda, Kiyotomi ^a  

^a OSAKA UNIVERSITY   (Japan)

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Indexed keywords

EID: 84855956919     PISSN: 03855414     EISSN: 18810942     Source Type: Journal    
DOI: 10.3987/COM-11-S(P)68     Document Type: Article

References (22)

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18. 4+-mont was prepared according to our previous report
19. 4+-mont (0.05 g). The reaction mixture was vigorously stirred at room temperature. The solid catalyst was removed by filtration and the yield was determined by GC analysis using an internal standard technique.
20. 4+-mont and molecular sieves were recovered by filtration, washed with 1,4-dioxane and dried at 110 oC in air for 3 h. Then, another portion of glycerol and carbonyl compounds were added, followed by stirring in the same manner as identical reaction conditions of the first run.
21. 4+-mont (0.5 g), glycerol (100 mmol) and acetone (300 mL) were placed in a flask. The reaction mixture was vigorously stirred at room temperature for 3 h. After the addition of magnesium sulfate, the mixture was filtered. The resulting filtrate was concentrated to afford 12.9 g of 1 (98% isolated yield) which was confirmed by GC.
22. 4+-mont (0.05 g), water (4 mL) and 1 (5 mmol) were placed in a Schlenk tube. The reaction mixture was vigorously stirred at room temperature for 24 h. The yield of glycerol was determined by GC analysis.