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CAS No. : | 16588-34-4 | MDL No. : | MFCD00007078 |
Formula : | C7H4ClNO3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | HETBKLHJEWXWBM-UHFFFAOYSA-N |
M.W : | 185.57 | Pubchem ID : | 85505 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H317-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 |
---|---|---|
98% | With sodium tetrahydroborate; ethanol; at 20℃; for 2h; | To a solution of 4-chloro-3-nitrobenzaldehyde (5.0 g, 27 mmol) in EtOH (100 mL) at rt was added portion wise NaBH4 (1.02 g, 1 eq). The mixture was stirred at RT for 2 h, concentrated in vacuo and partitioned between ether and water. The organic layer was washed with brine, dried over MgSO4 and concentrated. The title alcohol was recovered as a brownish solid (4.96 g, 98%).1H-NMR (CDCl3): δ=4.80 (s, 2H); 7.54 (m, 2H); 7.92 (s, 1H). |
98% | With sodium tetrahydroborate; In ethanol; at 20℃; for 2h; | To a solution of 4-chloro-3-nitrobenzaldehyde (5.0 g, 27 mmol) in EtOH (100 mL) at rt was added portion wise NaBH4 (1.02 g, 1 eq). The mixture was stirred at RT for 2h, concentrated in vacuo and partitioned between ether and water. The organic layer was washed with brine, dried over MgSO4 and concentrated. The title alcohol was recovered as a brownish solid(4.96g, 98%).1H-NMR (CDCl3): δ = 4.80 (s, 2H); 7.54 (m, 2H); 7.92 (s, IH). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
91% | With oxygen; sodium carbonate; In water; for 1.5h;Reflux; | General procedure: A mixture of alcohol (1 mmol), Na2CO3(2 mmol), and Fe3O4SiO2/CuO nanocatalyst (0.04 g) in water was stirred under oxygen at reflux condition. After reaction completion, the catalyst was separated from the reaction mixture by external magnetic field, washed with hot EtOAc (2 × 5 mL), and dried for consecutive reaction runs. Then, the filtrate was cooled to room temperature, quenched with 2 MHCl aqueous solution, filtered, and extracted with dichloromethane. The solvent was evaporated and the organic layer dried over anhydrous Na2SO4. Evaporation of the solvent followed by column chromatography on silica gel (n-hexane/ethyl acetate 9:1 as v/v%) afforded the pure products. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
48.5% | With sodium hydroxide; In (2S)-N-methyl-1-phenylpropan-2-amine hydrate; dichloromethane; water; | Step 1 Preparation of (Z)-3-(3-nitro-4-chlorophenyl)-2-(3,4,5-trimethoxyphenyl)-prop-2-ene-nitrile 5.0 g of 3-nitro-4-chlorobenzaldehyde, 5.6 g of <strong>[13338-63-1]3,4,5-trimethoxyphenylacetonitrile</strong>, 1.3 g of sodium hydroxide and 500 mg of trioctylmethylammonium chloride were dissolved in 10 ml of water and 50 ml of dichloromethane. The mixture was stirred vigorously for 3 hours at room temperature. The ice water was added to the mixture and the mixture was extracted with dichloromethane three times and dried over anhydrous sodium sulfate. The organic layer was concentrated and the residue was crystallized from ethyl acetate to give 4.9 g of the intended compound. The yield was 48.5%. 1 H-NMR(CDCl3): 8.23 (1H, J=2.1), 8.15 (1H, dd, J=2.1, 8.4), 7.67 (1H, d, J=8.4), 7.41 (1H, s), 6.88 (2H, s), 3.94 (6H, s), 3.91 (3H, s), mass spectrum (m/z): 374 (M+); melting point 198-199 C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
25% | General procedure: Trans-2-phenylcyclopropylamine hydrochloride (1.0 eq.), acetic acid (1.0eq.) and the appropriate aldehyde (0.9 eq.) were dissolved in around bottom flask in 10 mL dry DCE. The reaction mixture was stirred gently at room temperature for 2 h before sodium triacetoxyborohydride (3.0 eq.) was added in small portions to the reaction vessel. The reaction was monitored by TLC and quenched using 10 mL of an aqueous (5%) NaHCO3 solution. The organic layer was separated and the aqueous layer extracted three times with10 mL of DCE. All organic layers were combined, dried over anhydrous Na2SO4, concentrated in vacuo and purified using flash chromatography (silica gel; cyclohexane/ethyl acetate) to give the desired compound. |
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