4-BENZYL-2-HYDROXY-MORPHOLIN-3-ONE synthesis
- Product Name:4-BENZYL-2-HYDROXY-MORPHOLIN-3-ONE
- CAS Number:287930-73-8
- Molecular formula:C11H13NO3
- Molecular Weight:207.23
298-12-4
104-63-2
287930-73-8
A 50% aqueous solution of glyoxalate (67 mL, 0.61 mol) and tetrahydrofuran (130 mL) were added to a 250 mL round bottom flask and heated to reflux. A solution of N-benzylethanolamine (41.5 g, 0.27 mol) in tetrahydrofuran (20 mL) was slowly added dropwise under reflux conditions. After completion of the reaction, the tetrahydrofuran solvent was removed by rotary evaporator. Water (170 mL) was added to the residue, stirred and cooled to room temperature, followed by continued stirring in an ice water bath for 30 min to promote crystallization. The precipitated solid was collected by filtration and washed with ice water. The resulting pale yellow solid was dried to afford the target product 4-benzyl-2-hydroxy-morpholin-3-one (compound of formula VII, 51.8 g, 91% yield) with a melting point of 132-136 °C.
298-12-4
479 suppliers
$5.00/25g
104-63-2
359 suppliers
$7.00/10g
287930-73-8
220 suppliers
$6.00/5g
Yield:287930-73-8 91%
Reaction Conditions:
in tetrahydrofuranReflux;
Steps:
1
To a 250ml reaction flask was added 50% glyoxylic acid (67ml, 0.61mol) and tetrahydrofuran (130ml), heated to reflux, was added dropwise N- benzyl ethanolamine (41.5g, 0.27mol) in tetrahydrofuran (20ml) solution, to the reaction complete, the tetrahydrofuran was evaporated, water (170ml), cooled with stirring, to precipitate a solid, ice-water bath was stirred for 30 minutes, filtered and washed with ice water, drying in a yellowish solid, i.e. compounds of formula VII (51.8g, 91%), mp132 ~ 136 .
References:
Jiangsu Hansoh Pharmaceutical Ltd.;Xu, Shiwei;Yuan, Fuping CN103030668, 2016, B Location in patent:Paragraph 0031-0033
110843-90-8
23 suppliers
inquiry
287930-73-8
220 suppliers
$6.00/5g
104-63-2
359 suppliers
$7.00/10g
287930-73-8
220 suppliers
$6.00/5g
104-63-2
359 suppliers
$7.00/10g
563-96-2
308 suppliers
$6.00/25g
287930-73-8
220 suppliers
$6.00/5g