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CAS No. : | 118288-08-7 | MDL No. : | MFCD21607521 |
Formula : | C22H29N3O4S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 431.55 | Pubchem ID : | - |
Synonyms : |
FRG-8813;(+)-Lafutidine
|
Chemical Name : | (+)-(Z)-2-((Furan-2-ylmethyl)sulfinyl)-N-(4-((4-(piperidin-1-ylmethyl)pyridin-2-yl)oxy)but-2-en-1-yl)acetamide |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
87% | In Isopropyl acetate; at 35 - 40℃; for 5.0h; | 3) Transfer the above isopropyl acetate solution to a reaction flask, add 61 g of compound (III) and stir at 35-40 C for 5 hours.The reaction mixture was washed with 200 ml of 5% sodium hydroxide solution (twice), 200 ml of water at 20-30 C,After washing with 200 ml of 5% saline, it was dried over anhydrous sodium sulfate and filtered; 4) The filtrate was evaporated under reduced pressure at 40-50 C, and 100 ml of isopropyl ether was added.After stirring at 60 to 70 C for 30 minutes, slowly reduce the temperature to room temperature, and then stir at 5 to 10 C for half an hour, and filter; 5) The filter cake was dried under vacuum at 40-45 C for 10 hours to obtain 74 g of lafuridine; the yield was 87%; the purity was 99.86%; the total impurities were 0.14%; dihydrolafuridine was not detected. |
60% | In ethyl acetate; at 20℃; | prepared in the Example 2 enamine oil(compound of Formula 2) 13. 2g (0 · 05mol) was added 70mL of ethyl acetate, stirred to dissolve, then add 2-furyl-methanesulfonyl-nitrophenol acetate ester (formula 3 compound) 15. 6g (0. 05mol, HPLC purity 99.5%), the reaction mixture was stirred at room temperature for 3-4 hours, TLC the reaction was complete. Water was added 100mL, with concentrated hydrochloric acid to adjust PH 4, filtered, separated and the aqueous phase was added 150 mL of dichloromethane, potassium carbonate was added to the PH adjusted to about 10 and then separated and the aqueous layer was extracted 80mL of dichloromethane was added. The combined organic phases were washed with 30% potassium carbonate solution (100mLX4), washed with water (lOOmLX 5), the organic phase was separated, dried over anhydrous sodium sulfate, filtered, and concentrated to dryness, ethyl acetate was added 100mL, stirred at room temperature for crystallization , filtered crude, and then recrystallized from ethanol, active carbon, filtered hot, ice cooling crystallization, filtration, and dried to give a white solid 13. 5g, yield (calculated from the compound of formula 6) 60%, HPLC purity 99 88%. |