N-Acetyl-L-thioproline synthesis
- Product Name:N-Acetyl-L-thioproline
- CAS Number:54323-50-1
- Molecular formula:C6H9NO3S
- Molecular Weight:175.21
33898-90-7
34592-47-7
54323-50-1
GENERAL STEPS: L-thioproline (0.11 mol) and potassium chloride solution (100 mL) were added to the reaction vessel. The stirring speed was controlled at 150 rpm. the reaction mixture was heated to 85°C. A solution of 85% 2-thienylacetonitrile (50 mL) was slowly added dropwise with a controlled drip time of 40 min. The stirring rate was maintained and the reaction was continued for 120 minutes. Upon completion of the reaction, a reduced pressure distillation (2.3 kPa) was performed to separate the solid product. To the resulting solid, 90% p-xylene (80 mL) was added and heated to completely dissolve the solid. Decolorization was performed by adding decolorizing molecular sieves, maintaining the solution temperature at 15°C for 35 min. The solid impurities were removed by filtration and dehydrated using phosphorus pentoxide to give the final white N-acetyl-L-thioproline (1) (17.13 g, 89% yield).
33898-90-7
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$8.00/1g
34592-47-7
406 suppliers
$5.00/5g
54323-50-1
156 suppliers
$6.00/250mg
Yield:54323-50-1 89%
Reaction Conditions:
with potassium chloride at 85; for 2.66667 h;Temperature;
Steps:
3 Example 3
Into the reaction container, add L-thioproline 0.11mol, potassium chloride solution 100 ml. Control the stirring speed at 150rpm. The solution is heated up to 85 °C. Slowly add dropwise mass fraction of 85% 2-thenoylacetonitrile 50 ml. Add dropwise time controlled at 40 min. Maintain the stirring speed and maintain for 120 min. 2.3kPa reduced pressure distillation, to the solid separated out, by adding the mass fraction of 90% para-xylene 80 ml, heating the solid re-dissolved, decoloring molecular sieve for, maintaining the temperature of the solution 15 °C, for 35 min, filtering out the solid, phosphorus pentoxide dehydration, get white N-acetyl-L-thioproline (1) 17.13g, yield 89%.
References:
CN105541749,2016,A Location in patent:Paragraph 0014; 0015