D-Gluconic acid, 2,3,4-tris-O-(phenylmethyl)-, δ-lactone synthesis
- Product Name:D-Gluconic acid, 2,3,4-tris-O-(phenylmethyl)-, δ-lactone
- CAS Number:158464-67-6
- Molecular formula:C27H28O6
- Molecular Weight:448.52
13096-62-3
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Yield:158464-67-6 93 g
Reaction Conditions:
with sulfuric acid;acetic anhydride at 0; for 0.5 h;
Steps:
S2 S2, the synthesis of compound :
Add compound II (100.0g) to the reaction kettle, Acetic anhydride (500g) and sulfuric acid (1.0g), The control temperature is 0, HPLC monitoring started after 0.5h of reaction, The reaction ends when the content of compound II is ≤1.0%. After the reaction is over, slowly add the reaction solution to the water, Control the temperature at 30, stir for 30min, Extract once with ethyl acetate, Concentrate the organic phase under reduced pressure until there is no obvious fraction, Add ethanol (100g) and water (100g), reduce the temperature to 0, Add sodium hydroxide (20g) and raise the temperature to 30°C, Stir for 3h; then adjust the pH to 2 with 10% hydrochloric acid; Extract once with toluene and collect the organic phase; Concentrate the organic phase under reduced pressure until there is no obvious fraction, Compound III (93.0 g) was obtained.
References:
CN112645915,2021,A Location in patent:Paragraph 0065-0066
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