5,7-Dimethoxycoumarin synthesis
- Product Name:5,7-Dimethoxycoumarin
- CAS Number:487-06-9
- Molecular formula:C11H10O4
- Molecular Weight:206.19
708-76-9
181 suppliers
$7.00/100mg
105-58-8
481 suppliers
$14.00/25g
487-06-9
212 suppliers
$21.00/25mg
Yield:-
Reaction Conditions:
Stage #1:2-hydroxy-4,6-dimethoxybenzaldehyde;Diethyl carbonate with sodium hydride at 135; for 0.5 h;Reflux;
Stage #2: with hydrogenchloride in water; pH=5 - 6
Steps:
Step 1
2,4-Dimethoxy-6-hydroxybenzaldehyde (1, 5g, 1.0 eq.) was dissolved in 5 mL of dimethyl carbonate, and NaH (1.2 g, 1 2 eq.) was added The reaction mixture was refluxed at 135 °C for 30 mins. and then filtered to afford filter cake. The filter cake was dissolved in water, the pH was adjusted to 5-6 with aqueous 2M HCl to get a precipitate. The precipitated solid was collected by Alteration, and was redissolved in EtOAc. The solution was dried over anhydrous Na2S04, and filtered and the solvent was removed under reduced pressure to get the crude product 3, which was used as such for the next step.
References:
NEW YORK UNIVERSITY;THE GOVERNMENT OF THE UNITED STATES OF AMERICA AS REPRESENTED BY THE SECRETARY OF THE DEPARTMENT OF HEALTH AND HUMAN SERVICES;LITTMAN, Dan;HUH, Jun, R.;HUANG, Ruili;HUANG, Wenwei;ENGLUND, Erika, Elaine WO2013/36912, 2013, A2 Location in patent:Paragraph 00366
500-99-2
281 suppliers
$10.00/1g
471-25-0
235 suppliers
$10.00/1g
487-06-9
212 suppliers
$21.00/25mg
2732-18-5
105 suppliers
$16.00/100mg
74-88-4
357 suppliers
$15.00/10g
487-06-9
212 suppliers
$21.00/25mg
708-76-9
181 suppliers
$7.00/100mg
616-38-6
719 suppliers
$5.00/5 g
487-06-9
212 suppliers
$21.00/25mg
500-99-2
281 suppliers
$10.00/1g
15568-85-1
159 suppliers
$7.00/1g
487-06-9
212 suppliers
$21.00/25mg