Duloxetine iMpurity (alpha-hydroxy) synthesis
- Product Name:Duloxetine iMpurity (alpha-hydroxy)
- CAS Number:940291-11-2
- Molecular formula:C18H19NOS
- Molecular Weight:297.41
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Yield:-
Reaction Conditions:
with potassium hydroxide;water in 1-methoxy-2-propanol; for 96 h;Heating / reflux;
Steps:
1
Example 1 : Preparation of DLX-ISO-OH in PGME[0054] A 100 ml three necked flask equipped with a mechanical stirrer, thermometer, and condenser was charged with a mixture of 4.2 g of duloxetine in 42 ml PGME and 5.2 g of KOH (85%). The mixture was then heated to reflux and stirred for 96 hours.[0055] After cooling the mixture to room temperature, 50 ml of water and 50 ml of toluene were added, and the resulting organic phase was washed (4 x 50ml) with water, cooled to 00C and stirred for an additional hour, during which time DLX-ISO-OH precipitated. The DLX-ISO-OH was filtered from the water immiscible phase, washed with 20 ml of toluene, and dried in a vacuum oven at 50 C overnight.
References:
WO2007/67581,2007,A1 Location in patent:Page/Page column 11