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CAS No. : | 20440-95-3 | MDL No. : | MFCD00145004 |
Formula : | C20H19N | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | YWKKLBATUCJUHI-UHFFFAOYSA-N |
M.W : | 273.37 | Pubchem ID : | 88539 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
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 |
---|---|---|
31.5% | With trichlorophosphate; at 25 - 130℃; for 6h; | N,N-dimethylformamide (2.74 g, 37.5 mmol) was added dropwise to the mixture of TPA (2.27 g, 18.8 mmol) and phosphorous oxychloride (POCl3) (5.65 g, 22.5 mmol) at 25 °C. The reaction mixture was stirred and heated at 130 °C for 6 h. After cooling down to room temperature, the reaction mixture was poured into 50 mL cold water and extracted with chloroform (3 x 15 mL). The combined organic layer was dried with anhydrous MgSO4, filtered. The purified compound R2-CHO was obtained by recrystallizing from diluted ethanol. Yield: 1.75 g (31.5percent). Melting point: 96.3-97.5 °C. ESI-MS (m/z, [M + H]+)=302.4. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | With trichlorophosphate; In N,N-dimethyl-formamide; | 4-(Dip-tolylamino)benzaldehyde (H)N,N-dimethylformamide (6.0 ml) was charged in a two-necked bottle.The bottle was deoxygenated and purged with nitrogen, and added POCl3 (0.86 mL, 5.27 mmole) in an ice bath, and then stirred for 30 mins.Compound G was in DMF (6.0 ml) was added stepwise.The reaction was heated to 70° C., and stirred for 6 hours.The resulting was distilled to remove solvent under reduced pressure and the residue was purified by column chromatography (hexanes/CH2Cl2=6/1) to afford H (1.26 g, 95percent) as yellow solid.1H NMR (400 MHz, CDCl3): delta 9.75 (s, 1H), 7.62 (d, J=8.8 Hz, 2H), 7.13 (d, J=8.0 Hz, 4H), 7.05 (d, J=8.0 Hz, 4H), 6.92 (d, J=8.8 Hz, 2H), 2.33 (s, 6H).13C NMR (100 MHz, CDCl3): delta 190.4, 153.7, 143.5, 135.0, 131.3, 130.3, 128.3, 126.4, 118.2, 21.0.HRMS (m/z): [M+] calcd. for C21H19NO, 301.1467.Found, 301.1471. |