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CAS No. : | 174855-57-3 | MDL No. : | MFCD05864664 |
Formula : | C16H22N2O3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | FGJACYJASSSXNJ-UHFFFAOYSA-N |
M.W : | 290.36 | Pubchem ID : | 6490990 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H317-H319 | 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 |
---|---|---|
42.7% | With potassium carbonate; In dimethyl sulfoxide; at 130℃; for 4.0h;Inert atmosphere; | Put 2-fluorobenzaldehyde (4.0g, 32.2mmol),Piperazine-tert-butyl formate (6.6 g, 35.4 mmol) was added to DMSO (96 mL), followed by potassium carbonate (6.4 g, 64.4 mmol). The reaction was heated to 130 C. for 4 hours under nitrogen protection. The reaction was stopped and cooled to room temperature. The reaction solution was quenched with water (100 mL), extracted with ethyl acetate (60 mL × 3), and the organic phase was collected, washed with water and saturated brine in sequence, dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The obtained crude product was subjected to silica gel chromatography. Column (petroleum ether: ethyl acetate (V: V) = 10: 1) was further purified to give the title compound (light yellow solid, 4.0 g, 42.7%). |
8.5 g | With potassium carbonate; In dimethyl sulfoxide; at 100℃; for 12.0h; | To a solution of 2-fluorobenzaldehyde (13.33 g, 107.38 mmol) and tert-butyl piperazine-1-carboxylate (30.0 g, 161.07 mmol) in DMSO (150 mL) was added K 2CO 3 (44.52 g, 322.15 mmol). The mixture was stirred at 100C for 12 hr. TLC indicated the reactant was consumed completely. The reaction mixture was cooled to room temperature and poured into H 2O (150 mL) and extracted with EA (150 mL 3), dried over Na 2SO 4, filtered and concentrated. The residue was purified by column chromatography (Silica gel, PE/EA=100/1 to 30/1). Tert-butyl 4- (2-formylphenyl) piperazine-1-carboxylate (8.5 g) was obtained as a yellow solid. 1H NMR (400MHz, CDCl 3) δ ppm: 1.50 (s, 9 H), 3.02 -3.08 (m, 4 H), 3.61 -3.66 (m, 4 H), 7.11 (d, J=8.2 Hz, 1H), 7.17 (t, J=7.5 Hz, 1H), 7.52 -7.58 (m, 1H), 7.83 (dd, J=7.7, 1.8 Hz, 1H), 10.36 (s, 1H). |
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