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CAS No. : | 21803-75-8 | MDL No. : | MFCD00052917 |
Formula : | C7H5ClN2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | OREVCMGFYSUYPX-UHFFFAOYSA-N |
M.W : | 152.58 | Pubchem ID : | 519896 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | 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 |
---|---|---|
74% | With sodium borate; In acetic acid; at 50 - 62℃; for 3h; | A suspension of sodium borate tetrahydrate (32.5 g, 211.2 mmol) in 195 ml of acetic acid was heated until the temperature of the reaction mixture was above 50 C. The reaction temperature was kept this way while 2-chloro-4-cyanoaniline (5.93 g, 38.9 mmol) was added in portions over 1 h. Stirring and heating were continued for 2 hours on an oil bath of 62 C. After cooling to room temperature the reaction mixture was poured into 1 L icewater. The aqueous layer was extracted with Et2O (3×). The combined organic layers were washed with H2O (2×) and dried (MgSO4). The drying agent was removed by filtration and the solvent by evaporation under reduced pressure. The residue was chromatographed (SiO2) with Et2O/petroleum ether 1/3 as eluent to give 5.27 g (74%) of the oxidized product. |
With sodium nitrite; In hydrogenchloride; water; | 1. 4-nitro-3-chlorobenzonitrile To an ice cold solution of 4-amino-3-chlorobenzonitrile (1 g, 6.6 mmol) in concentrated HCl (2.5 mL) plus water (2.5 mL) a chilled solution of sodium nitrite (0.74 g, 1.62 eq) in water (3.6 mL) is added dropwise to maintain the reaction temperature <0 C. After stirring at 0 C. for 10 min, the mixture is added portion-wise to an ice cold solution of sodium nitrite (3.29 g, 7.22 eq) and copper(I) oxide (349 mg, 0.37 eq) in water 14.5 mL). Stirring is continued at 0 C. for 40 min, and then at room temperature for 0.5 h. The reaction mixture is extracted with dichloromethane (2*), the combined organic layers washed with saturated aqueous sodium chloride, dried (MgSO4), concentrated, and purified by silica gel chromatography to give 4-nitro-3-chlorobenzonitrile. 1H NMR (CDCl3): delta 7.96 (d, J=8.24 Hz, 1 h), 7.88 (d, J=1.65 Hz, 1H), 7.63 (dd, J=1.65, 8.24 Hz, 1H. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogenchloride; sodium nitrite; In water; | 3-Chloro-4-nitro-benzonitrile Sodium nitrite (6.78 g in water (40 mL) at 0 C.) was slowly added to a solution of 4-amino-3-chloro-benzonitrile (10.5 g) in water (30 mL) and concentrated hydrochloric acid (30 mL) also at 0 C. After 10 minutes the solution was poured onto a suspension of cuprous oxide (3.48 g) and sodium nitrite (31.69 g) in water (100 mL) at 0 C. The ensuing mixture was stirred at 0 C. for 1 hour then at 23 C. for 1 hour. The resulting mixture was extracted with dichloromethane and the organic layer washed with saturated sodium chloride. The separated organic layer was dried over sodium sulfate and then concentrated to give 3-chloro-4-nitro-benzonitrile (11.31 g). |
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