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CAS No. : | 1192-58-1 | MDL No. : | MFCD00003087 |
Formula : | C6H7NO | Boiling Point : | - |
Linear Structure Formula : | CH3C4H3NCHO | InChI Key : | OUKQTRFCDKSEPL-UHFFFAOYSA-N |
M.W : | 109.13 | Pubchem ID : | 14504 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H227-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 |
---|---|---|
68% | With acetic acid;Reflux; | General procedure: A solution of 1 (0.93 g, 5 mmol) and the appropriate aldehyde (5 mmol) in gl. acetic acid (15 mL) was refluxed for 6-8 h. The solid product separated upon cooling was filtered, washed with cold ethanol, dried and recrystallized. Physicochemical and analytical data are recorded in Table 3. IR (cm-1): 1690 - 1675 (C=O), 1640 - 1630 (C=N). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
23% | A 100mL round-bottomed flask was charged with <strong>[6882-68-4]sophoridine</strong> (1.24g, 5mmol), NaH (2.4g, 100mmol) and 50mL anhydrous tetrahydrofuran. The solution was stirred at room temperature for 1h and then N-substituted pyrrole-2-carboxyaldehyde 2 (2a-2u) (5mmol) was added followed by reflux for 48h. Reaction mixture was cooled and poured into water slowly (100mL). Reaction mixture was then extracted with dichloromethane (3×40mL). The organic phase was dried with anhydrous Na2SO4 and concentrated to give crude product. The residue was purified by silica gel flash column chromatography (methanol/dichloromethane, 1%) to afford 3a-3u in 23%-54% yields. | |
23% | With sodium hydride; In tetrahydrofuran; at 85℃; for 36h; | 2.4 g (100 mmol) of sodium hydride and 50 mL of anhydrous tetrahydrofuran were added to a 100 mL round bottom flask.Stir well, add 1.24 g (5 mmol) of <strong>[6882-68-4]sophoridine</strong>, slowly warm to 85 C, add 0.654 g (6 mmol) of N-methyl-2-pyrrolidine, and react for 36 h to the end point (TLC detection).After cooling to room temperature, excess sodium hydride was neutralized by dropwise addition of 3N hydrochloric acid.Dichloromethane extraction (40 mL×3), the organic phase was combined, dried over anhydrous Na2SO4.(V dichloromethane: V methanol = 50:1) was purified to give 0.389 g of light brown solid powder LYL-01: 14-(N-methyl-2-pyrrol-2-ylmethylene)<strong>[6882-68-4]sophoridine</strong>: yield 23%; |
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