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ChemicalBook CAS DataBase List trans-2-isopropyl-5-carboxy-1,3-dioxane
42031-28-7

trans-2-isopropyl-5-carboxy-1,3-dioxane synthesis

2synthesis methods
-

Yield:89.848 % de

Reaction Conditions:

with 4-methyl-morpholine in acetonitrile at 80 - 105; for 4 h;Overall yield = 72.8 %; Overall yield = 5.75 g;Solvent;Reagent/catalyst;

Steps:

5 Example 5

2-isopropyl-5,5-dicarboxy-1,3-dioxane 10.0 g (0.046 mol),N-methylmorpholine 4.6g(0.046 mol) was added to 100 mL of acetonitrile, heated to 80-105 ° C, reacted for 4 h, and monitored by HPLC until the reaction of the starting material was complete, and the addition was stopped.Heat, remove the solvent under reduced pressure at 50 ° C, add purified water to cool to about 5 ° C, adjust the pH value of about 2.5 with 1 mol / L hydrochloric acid, to protectStirring at a temperature of 5 ° C for 1 h, suction filtration, and drying at about 50 ° C to obtain the product 2-isopropyl-5-carboxy-1,3-dioxane5.75 g, the yield was 72.8%, and the ratio of the cis-trans configuration of HPLC was 1:18.7.

References:

CN108929304,2018,A Location in patent:Paragraph 0028; 0029; 0038-0046