Preparation of cholecystokinin octapeptide
A technology of cholecystokinin and a condensation reagent, applied in the field of polypeptide chemistry, can solve the problems of easy decomposition of products, long cycle, complicated preparation process of sincalide, etc., and achieves low-toxicity and pollution-free reagents, mild conditions and short preparation cycle. Effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0024] Embodiment 1: Preparation of sincalide
[0025] (1) Preparation of protected sincalide-resin complexes
[0026] Add 1g of Wang resin (1.0mmol / g) into the reactor with filter device, inject 10ml of DMF, let stand for 1h, and filter.
[0027] Take 4mmol Fmoc-Phe-OH, 4mmol DIC, 3mmol HOBt and 0.5mmol DMAP, dissolve in 10ml DMF, then add the resulting solution into the reactor, and react at 20°C for 5h. After the reaction, filter. Then 10ml of DMF was added, the resin was washed three times and filtered.
[0028] Add 10ml of 20% v / v PIP and DMF mixed solution into the reactor, and react at 20°C for 0.5h. After the reaction is complete, filter. Then add 10ml DMF to wash the resin three times and filter.
[0029] Take 3mmol Fmoc-Asp(ODmab)-OH, 3mmol HBTU, 3mmol HOBt and 6mmol DIEA, dissolve in 10ml DMF, add the resulting solution into the reactor, and react at 20°C for 1h. After the reaction, filter. Then 10ml of DMF was added, the resin was washed three times and filt...
Embodiment 2
[0037] Embodiment 2: Preparation of sincalide
[0038] (1) Preparation of protected sincalide-resin complexes
[0039] Add 2g of Pam resin (1.0mmol / g) into the reactor with filter device, inject 15ml of DMF, let stand for 1h, and filter.
[0040] Take 8mmol Fmoc-Phe-OH, 8mmol DIC, 6mmol HOBt and 1mmol DMAP, dissolve in 10ml DMF, then add the resulting solution into the reactor, and react at 20°C for 5h. After the reaction, filter. Then 15ml of DMF was added, the resin was washed three times and filtered.
[0041] Add 15ml of 20% v / v PIP and DMF mixed solution into the reactor, and react at 20°C for 0.5h. After the reaction is complete, filter. Then add 15ml DMF to wash the resin three times and filter.
[0042] Take 6mmol Fmoc-Asp(ODmab)-OH, 6mmol HBTU, 6mmol HOBt and 12mmol DIEA, dissolve in 15ml DMF, add the resulting solution into the reactor, and react at 20°C for 1h. After the reaction, filter. Then 15ml of DMF was added, the resin was washed three times and filtered...
Embodiment 3
[0050] Embodiment 3: Preparation of sincalide
[0051] (1) Preparation of protected sincalide-resin complexes
[0052] Add 3g of Hydromethyl resin (1.0mmol / g) into the reactor with filter device, inject 20ml of DMF, let stand for 1h, and filter.
[0053] Take 12mmol Fmoc-Phe-OH, 12mmol DIC, 9mmol HOBt and 1.5mmol DMAP, dissolve in 20ml DMF, then add the resulting solution into the reactor, and react at 20°C for 5h. After the reaction, filter. Then add 20ml of DMF, wash the resin three times, and filter.
[0054] Add 20ml of 20% v / v PIP and DMF mixed solution into the reactor, react at 20°C for 0.5h. After the reaction is complete, filter. Then add 20ml DMF to wash the resin three times and filter.
[0055] Take 9mmol Fmoc-Asp(ODmab)-OH, 9mmol HBTU, 9mmol HOBt and 18mmol DIEA, dissolve in 20ml DMF, add the resulting solution into the reactor, and react at 20°C for 1h. After the reaction, filter. Then add 20ml of DMF, wash the resin three times, and filter.
[0056] Acco...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More