Preparation method and application of monobutyryl cyclic adenosine monophosphate or its salt
A technology for monobutyryl cycloadenosine monophosphate and cycloadenosine monophosphate, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve problems such as reports, preparation of monobutyryl cycloadenosine monophosphate and structure confirmation, etc. Achieving the effect of good process, control of drug quality and simple operation
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0036] Preparation of monobutyryl cyclic adenosine monophosphate
[0037] Take 10g of cyclic adenosine monophosphate and place it in a 1000mL three-necked flask, add 600mL of tetrahydrofuran under nitrogen protection and stir to dissolve, then add 40mL of n-butyric anhydride and 5mL of N,N-diisopropylethylamine, and react in the dark at 50°C for 48 hours , lowered to room temperature, added water for hydrolysis for 1 hour, concentrated under reduced pressure at 35°C to remove tetrahydrofuran, added water to 500 mL, washed the water phase twice with methyl tert-butyl ether, 100 mL each time, washed the water phase twice with methyl ethyl ketone, each time 100mL, wash the water phase twice with dichloromethane, 300mL each time, distill the water phase under reduced pressure at 50°C, then extract the remaining water phase with dichloromethane for 3 times, 100mL each time, combine the organic phases, and remove the dichloromethane under reduced pressure , Obtained 7.6 g of slightl...
Embodiment 2
[0044] Preparation of barium monobutyryl cycloadenosine monophosphate
[0045] Take 10g of cyclic adenosine monophosphate and place it in a 1000mL three-neck flask, add 500mL of pyridine under the protection of helium and stir to dissolve, then add 50mL of n-butyric anhydride and 5mL of triethylamine, react in the dark at 80°C for 25 hours, cool to room temperature, add water Hydrolyze for 1 hour, concentrate under reduced pressure at 45°C to remove pyridine, add water to 400mL, wash the aqueous phase twice with methyl tert-butyl ether, 100mL each time, wash the aqueous phase twice with butanone, 100mL each time, wash with dichloromethane Wash the water phase twice, 300 mL each time, distill the water phase at 60 °C under reduced pressure, then extract the remaining water phase with dichloromethane 3 times, 100 mL each time, combine the organic phases, remove the dichloromethane under reduced pressure, and obtain slightly viscous light Yellow monobutyryl cyclic adenosine monop...
Embodiment 3
[0048] Preparation of sodium monobutyryl cyclic adenosine monophosphate
[0049] Take 20g of cyclic adenosine monophosphate and place it in a 1000mL three-necked flask, add 600mL tetrahydrofuran under nitrogen protection and stir to dissolve, then add 80mL n-butyric anhydride, 10mL triethylamine, react at 65°C for 30 hours in the dark, cool down to room temperature, add water for hydrolysis Concentrate under reduced pressure at 35°C for 3 hours to remove tetrahydrofuran, add water to 1800 mL, wash the aqueous phase twice with methyl tert-butyl ether, 1000 mL each time, wash the aqueous phase twice with methyl ethyl ketone, 1000 mL each time, and wash with dichloromethane The water phase was distilled at 60°C under reduced pressure for 2 times, 600 mL each time, and the remaining water phase was extracted 3 times with dichloromethane, 200 mL each time, the organic phase was combined, and the dichloromethane was removed under reduced pressure to obtain slightly viscous light yell...
PUM
| Property | Measurement | Unit |
|---|---|---|
| Elution gradient | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More