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CAS No. : | 599-04-2 | MDL No. : | MFCD00005392 |
Formula : | C6H10O3 | Boiling Point : | - |
Linear Structure Formula : | (CH3)2CCH2OC(O)CH(OH) | InChI Key : | SERHXTVXHNVDKA-BYPYZUCNSA-N |
M.W : | 130.14 | Pubchem ID : | 439368 |
Synonyms : |
D-(-)-Pantolactone
|
Chemical Name : | (R)-3-Hydroxy-4,4-dimethyldihydrofuran-2(3H)-one |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | With triethylamine; In ethanol; at 160℃; for 3.0h;Microwave irradiation; | Step 1 : (R)-2, 4-Dihydroxy-N-(3-hydroxy-propyl)-3, 3-dimethyl-butyramideTo a solution of D-pantolactone (0.5 g, 1 eq) in dry EtOH (5 mL) in a microwave vial were added 3-amino-propan-1-ol (0.53 mL, 1.5 eq), Et3N (0.54 mL, 1 eq) and irradiated with MW radiation at 160C for 3 h. After this time, the reaction mixture wasconcentrated and purified by silica gel column chromatography to afford the product as a white solid (800 mg, 95%).1H NMR (400 MHz, DMSO d6): delta 7.70 (t, J = 4.0 Hz, 1 H), 5.32 (d, J = 4.0 Hz, H), 4.48-4.42 (m, 2H), 3.68 (d, J = 8.0 Hz, 1 H), 3.40 (dd, J = 4.0, 8.0 Hz, 2H), 3.31-3.26 (m, 1 H), 3.19-3.07 (m, 3H), 2.56-2.52 (m, 2H), 0.78 (s, 3H), 0.76 (s, 3H). |
at 60℃; for 5.0h; | Preparation of Panthenol:A 1 l four-neck flask was initially charged with 150 g of 3-aminopropanol. While stirring, 260 g of D-pantolactone were added slowly at room temperature. After the addition had ended, the reaction mixture was heated to 60 C. and stirred for a further 5 hours. The D-pantolactone used was washed twice beforehand with methyl tert-butyl ether (MTBE) and then dried.The crude panthenol obtained by the reaction of 3-aminopropanol and D-pantolactone was subsequently degassed and distilled.The degassing was performed in a thin-film evaporator at a pressure of 0.027 mbar, a bottom temperature of 80 C. and a lamellar speed of 280 rpm. After the degassing, the apparatus was cleaned by repeatedly purging with demineralized water and 2-propanol with subsequent drying under reduced pressure.Subsequently, the degassed panthenol was distilled. The distillation was performed in the same apparatus in which the degassing had already been undertaken. The bottom temperature was 120 C., the pressure 0.027 mbar and the lamellar speed 800 rpm.In the internal condenser, at a cooling coil temperature of 60 C., panthenol was obtained. |
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