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CAS No. : | 125652-55-3 | MDL No. : | MFCD08458942 |
Formula : | C10H16ClN | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | PHCASOSWUQOQAG-UHFFFAOYSA-M |
M.W : | 185.69 | Pubchem ID : | 19876500 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P264-P280-P302+P352+P332+P313+P362+P364-P305+P351+P338+P337+P313 | UN#: | |
Hazard Statements: | H315-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 |
---|---|---|
In toluene; at 20 - 130℃;Inert atmosphere; | General procedure: The used method was modified to increase the product yield: alkyl halide (0.2000 mol) was added into two-neck round-bottom flask with the solution of 3-substituted pyridine (0.1665 mol) in toluene (20 ml). The solution was then stirred using a magnetic stirrer under a nitrogen atmosphere for 1 h at room temperature. After that the reaction mixture has been stirred at 110-130 C for 24-48 h to reflux condenser plant without access to nitrogen. After the reaction completion the obtained product delaminated; the dense layer of ionic liquid was decanted from the toluene layer. The product was washed with toluene. Recrystallization was carried out by dissolution in acetonitrile followed by precipitation in excess of diethyl ether. Volatile organic compounds have been removed for 6-8 h using the rotary evaporator (Rotavapor R-215, Buechi), at pressure gradual decrease from atmospheric one to 20-120 mbar, and temperature rise from 60 C to 90-140 C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
, wherein said salt is selected from the group consisting of: ... 1-decyl-3-methylimidazolium bromide, 1-dodecyl-3-methylimidazolium chloride, 1-methyl-3-tetradecylimidazolium chloride, 4-methyl-N-butylpyridinium chloride, 3-methyl-N-butylpyridinium chloride, 4-methyl-N-hexylpyridinium chloride, 1-ethyl-3-methylimidazolium tetrafluoroborate, 1-butyl-3-methylimidazolium tetrafluoroborate, ... |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
91% | With water; | 8.08 g (62.7 mmol) K[BH(CN)3] dissolved in 35 cm3 of water and 11.63 g (62.6 mmol) of <strong>[125652-55-3]1-butyl-3-methylpyridinium chloride</strong>, [BMPy]CI, dissolved in 18 cm3 of water are mixed together at room temperature. The product, 1- butyl-3-methylpyridinium tricyanohydridoborate is extracted with dichloromethane (100 + 50 + 50 cm3 of CH2CI2). The organic phase is washed two times with water (50 + 50 cm3) and dried with Na2S0 . The solvent is distilled off and the residue is dried in vacuum at ca. 40 C for one day. The yield of liquid at room temperature1-butyl-3-methylpyridinium tricyanohydridoborate, [BMPy] [BH(CN)3], is 13.64 g (91%).1H-NMR (Solvent: Aceton-D6): delta, ppm = 0.991 (CH3> 3H), 3JH,H = 7.5 Hz; 1.45 m (CH2l 2H); 1.74 d (1 H, BH), 1JH.B = 97 Hz; 2.09 m (CH2, 2H); 2.63 s (CH3, 3H), 4.72 t (CH2, 2H), 3JH,H = 7.6 Hz; 8.10 d,d (CH, 1H), 3JH,H = 7.0 Hz; 8.50 d (CH, 1H), 3JH,H = 8.0 Hz; 8.88 d (CH, 1H), 3JH,H = 6.1 Hz; 8.94 s (CH. 1 H).11B-NMR (Solvent: Aceton-D6): o~, ppm = -40.1 d, 1JB,H = 97 Hz. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
90% | In water; | Example 91-Butyl-3-methylpyridinium dicyanodihydridoborate-[BMPy][BH2(CN)2]4.09 g (46.6 mmol) of sodium dicyanodihydridoborate, Na[BH2(CN)2], and 8.63 g (46.5 mmol) of <strong>[125652-55-3]1-butyl-3-methylpyridinium chloride</strong>, [BMPy]Cl, are each dissolved in 20 ml of water and mixed. The product, 1-butyl-3-methylpyridinium dicyanodihydridoborate, [BMPy][BH2(CN)2], is extracted with 100+100+50 ml of CH2Cl2. The combined organic phases are washed with 50+50 ml of water, dried using Na2SO4, and the solvent is distilled off. [BMPy][BH2(CN)2] is dried at about 40 C. in vacuo for one day with stirring. The yield of 1-butyl-3-methylpyridinium dicyanodihydridoborate is 9.0 g (41.8 mol, 90%). 1H{11B}-NMR (solvent: acetone-D6; reference: TMS): delta, ppm=0.97 t (CH3, 3H), 3JH,H=7.5 Hz; 1.02 s (2H, BH2); 1.44 m (CH2, 2H); 2.08 m (CH2, 2H); 2.63 s (CH3, 3H), 4.71 t (CH2, 2H), 3JH,H=7.6 Hz; 8.08 d, d (CH, 1H), 3JH,H=7.0 Hz; 8.50 d (CH, 1H), 3JH,H=8.1 Hz; 8.88 d (CH, 1H), 3JH,H=6.1 Hz; 8.95 s (CH, 1H). 11B{1H}NMR (solvent: acetone-D6; reference: Et2O.BF3): delta, ppm=-41.7 s |
With sodium sulfate; In water; | Example 9 1-Butyl-3-methylpyridinium dicyanodihydridoborate-[BMPy][BH2(CN)2] 4.09 g (46.6 mmol) of sodium dicyanodihydridoborate, Na[BH2(CN)2], and 8.63 g (46.5 mmol) of <strong>[125652-55-3]1-butyl-3-methylpyridinium chloride</strong>, [BMPy]Cl, are each dissolved in 20 ml of water and mixed. The product, 1-butyl-3-methylpyridinium dicyanodihydridoborate, [BMPy][BH2(CN)2], is extracted with 100+100+50 ml of CH2Cl2. The combined organic phases are washed with 50+50 ml of water, dried using Na2SO4, and the solvent is distilled off. [BMPy][BH2(CN)2] is dried at about 40 C. in vacuo for one day with stirring. The yield of 1-butyl-3-methylpyridinium dicyanodihydridoborate is 9.0 g (41.8 mol, 90%). 1H{11B}-NMR (solvent: acetone-D6; reference: TMS): delta, ppm=0.97 t (CH3, 3H), 3JH,H=7.5 Hz; 1.02 s (2H, BH2); 1.44 m (CH2, 2H); 2.08 m (CH2, 2H); 2.63 s (CH3, 3H), 4.71 t (CH2, 2H), 3JH,H=7.6 Hz; 8.08 d, d (CH, 1H), 3JH,H=7.0 Hz; 8.50 d (CH, 1H), 3JH,H=8.1 Hz; 8.88 d (CH, 1H), 3JH,H=6.1 Hz; 8.95 s (CH, 1H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98% | With Iodine monochloride; In dichloromethane; water; at 0 - 20℃; for 1.0h; | A black solution of ICl (3.14g, 19.39 mmol) in dichloromethane (35ml) was added drop wise to an ice cold solution of <strong>[125652-55-3]1-butyl-3-methylpyridinium chloride</strong> (3.0g, 16.16 mmol) in water (16ml) under stirring and then left to attain room temperature. After the reaction mixture was stirred for 1 hour, the dichloromethane layer was separated and dried with sodium sulfate and then evaporated under vacuum to afford water soluble dark reddish brown ionic liquid 1-butyl-3-methylpyridinium dichloroiodate (BMPDCI) in quantitative yields (5.5g, 98%). This ionic liquid was stable and stored in dark at 10 C (in refrigerator) for several months without any change in colour, loss of reactivity and degradation (checked by NMR). 1H NMR (200 MHz, DMSO-d6 delta/ppm): 9.03 (s, 1H, Ar-H), 8.97 (d, 1H, 7=5.94 Hz, Ar-H), 8.51 (d, 1H, 7=7.96 Hz, Ar-H), 8.10 (dd, 1H, 7=1.37 Hz, 8.42 Hz, Ar-H), 4.59 (t, 2H, CH2), 2.56 (s, 3H, Ar-CH3), 2.03-1.88 (m, 2H, -CH2-CH2), 1.40-1.29 (m, 2H, CH2-CH3) 0.97 (t, 3H,CH3). 13C NMR (50 MHz, CDCl3+DMS0-d6): 12.23, 17.50, 18.13, 32.17, 60.56, 126.69, 138.72, 140.57, 142.91, 144.88. |