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CAS No. : | 50995-74-9 | MDL No. : | MFCD00068721 |
Formula : | C14H15NO4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | WHCPTFFIERCDSB-UHFFFAOYSA-N |
M.W : | 261.27 | Pubchem ID : | 659294 |
Synonyms : |
DEAC;Coumarin D 1421;7-Diethylamino-2-oxo-2H-chromen-3-carboxylic Acid;7-DCCA;7-(Diethylamino)coumarin-3-carboxylic Acid;D 1421
|
Chemical Name : | 7-(Diethylamino)-2-oxo-2H-chromene-3-carboxylic acid |
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 |
---|---|---|
67% | With pyridine; trichlorophosphate; | General procedure: Intermediate 4 (0.001mol) and 5 (0.001mol) were dissolved in pyridine, phosphorus oxychloride is slowly added dropwise under ice bath conditions, then at 40-60C reacted for 5-8h. Finally, the mixture was poured into 30mL saturated Na2CO3 solution and stirred well. After the mixture was acidified, the saturated CuSO4 solution was used to remove pyridine, which greatly improved the purity and yield of the product. The data for compounds 8I-8VI are provided in the supporting information. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | With pyridine; trichlorophosphate; | General procedure: Intermediate 4 (0.001mol) and 5 (0.001mol) were dissolved in pyridine, phosphorus oxychloride is slowly added dropwise under ice bath conditions, then at 40-60C reacted for 5-8h. Finally, the mixture was poured into 30mL saturated Na2CO3 solution and stirred well. After the mixture was acidified, the saturated CuSO4 solution was used to remove pyridine, which greatly improved the purity and yield of the product. The data for compounds 8I-8VI are provided in the supporting information. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | With pyridine; trichlorophosphate; | General procedure: Intermediate 4 (0.001mol) and 5 (0.001mol) were dissolved in pyridine, phosphorus oxychloride is slowly added dropwise under ice bath conditions, then at 40-60C reacted for 5-8h. Finally, the mixture was poured into 30mL saturated Na2CO3 solution and stirred well. After the mixture was acidified, the saturated CuSO4 solution was used to remove pyridine, which greatly improved the purity and yield of the product. The data for compounds 8I-8VI are provided in the supporting information. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | With pyridine; trichlorophosphate; | General procedure: Intermediate 4 (0.001mol) and 5 (0.001mol) were dissolved in pyridine, phosphorus oxychloride is slowly added dropwise under ice bath conditions, then at 40?60°C reacted for 5?8h. Finally, the mixture was poured into 30mL saturated Na2CO3 solution and stirred well. After the mixture was acidified, the saturated CuSO4 solution was used to remove pyridine, which greatly improved the purity and yield of the product. The data for compounds 8I-8VI are provided in the supporting information. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
3.9% | A dimethylformamide solution of 7-(diethylamino)coumarine-3-carboxylic acid (70 mg, 0.27 mmol), dicyclohexylcarbodiimide(110 mg, 0.53 mmol), and 1-hydroxybenzotriazole(72 mg, 0.53 mmol) was stirred at 0 °C for30 min. To the mixture was added 6-deoxy-6-amino-beta-CD(250 mg, 0.22 mmol). The resulting solution was stirredat 0 °C for 5 h and subsequently at room temperature for 3days. After removing insoluble materials by filtration, thefiltrate was concentrated, and poured into acetone (500 mL)to form precipitates. The precipitate containing the productwas purified by column chromatography on high porouspolystylene gel, DIAION HP-20. The eluent with a 30percent methanol aqueous solution was concentrated to give thedesired product as a pale yellow solid (12 mg 3.9percent). Thepurity of the product was checked with TLC, 1H NMR, andelemental analysis. |