问题描述:
求翻译,希望大家帮忙.不要工具翻的,谢谢啦!
In a flask fitted with a reflux condenser were added 1.00 g
(10.4 mmol) of 1,2-dimethylimidazole and 1.43 g (10.4 mmol)
of butyl bromide. After addition, the mixture was stirred at
140 ◦C during 1 h to give a white solid. This solid was recrystallized
from acetonitrile and dried under reduced pressure to give
2.29 g (95% yield) of BMMIBr as white crystals. In another
flask, 250 mg (1.07 mmol) of BMMIBr were placed and dissolved
in 5.0mL of water followed by an aqueous solution
of LiTFSI (308 mg, 1.07 mmol) in 5.0mL of water. The reaction
mixture was stirred overnight at room temperature and two
phases were formed and separated. The phase containing the
ionic liquid was washed several times with water, treated with
activated carbon and subjected to a chromatography column
(alumina, dichloromethane). The ionic liquid was dried under
reduced pressure during 3 days at 100 ◦C to give BMMITFSI as
a colorless liquid (301 mg, 0.70 mmol, 65% yield).
BMPTFSI and BMITFSI were also synthesized following
the above procedure. BMIBr was obtained as a white solid after
recrystallization from tetrahydrofuran instead of acetonitrile. All
ionic liquids were stored in an argon atmosphere glove-box Labmaster
130 (H2OandO2 < 1 ppm) and all samples were prepared
and sealed in the glove-box to avoid water contamination. The
water contain of both RTILs was measured using the standard
Karl–Fischer method and it was estimated to be below 30 ppm.
The structures of the bromide derivatives and of the ionic liquids
were identified by 1H and 13C NMR, FTIR and elemental
analysis. The results for BMMI and BMP salts are summarized
below. The BMITFSI data are not shown here due to extensive
literature data available [64–68]. It is important to note that the
yields obtained in both cases are lower than those reported by
Appetecchi et al. [69]. These differences could be assigned to
the use of bromide instead of iodine derivatives and also to the
loss of material during the purification processes.
BMMIBr data—mp 95–97 ◦C; found: C, 46.22; H, 6.96.
Calc for C9H17BrN2: C, 46.36; H, 7.35; νmax(KBr), cm−1:
3129, 3078, 2961, 2933, 2873, 1588, 1538, 1517, 1466, 1380,
1251 and 1136; δH (300 MHz, CDCl3, ppm): 0.97 (3H, t,
CH2CH2CH2CH3, J = 7 Hz), 1.40 (2H, m, CH2CH2CH2CH3),
1.81 (2H, m, CH2CH2CH2CH3), 2.83 (3H, s, CH3), 4.04 (3H,
s, NCH3), 4.25 (2H, t, CH2CH2CH2CH3, J = 7 Hz), 7.58 (1H,
d, CHring, J = 2.1 Hz) and 7.77 (1H, d, CHring, J = 2.1 Hz); δC
(75 MHz, CDCl3, ppm): 11.0, 13.6, 19.6, 31.8, 36.2, 48.8, 121.3,
123.1 and 143.7.
如果用软件翻译的麻烦别贴啦!
谢谢啦!
In a flask fitted with a reflux condenser were added 1.00 g
(10.4 mmol) of 1,2-dimethylimidazole and 1.43 g (10.4 mmol)
of butyl bromide. After addition, the mixture was stirred at
140 ◦C during 1 h to give a white solid. This solid was recrystallized
from acetonitrile and dried under reduced pressure to give
2.29 g (95% yield) of BMMIBr as white crystals. In another
flask, 250 mg (1.07 mmol) of BMMIBr were placed and dissolved
in 5.0mL of water followed by an aqueous solution
of LiTFSI (308 mg, 1.07 mmol) in 5.0mL of water. The reaction
mixture was stirred overnight at room temperature and two
phases were formed and separated. The phase containing the
ionic liquid was washed several times with water, treated with
activated carbon and subjected to a chromatography column
(alumina, dichloromethane). The ionic liquid was dried under
reduced pressure during 3 days at 100 ◦C to give BMMITFSI as
a colorless liquid (301 mg, 0.70 mmol, 65% yield).
BMPTFSI and BMITFSI were also synthesized following
the above procedure. BMIBr was obtained as a white solid after
recrystallization from tetrahydrofuran instead of acetonitrile. All
ionic liquids were stored in an argon atmosphere glove-box Labmaster
130 (H2OandO2 < 1 ppm) and all samples were prepared
and sealed in the glove-box to avoid water contamination. The
water contain of both RTILs was measured using the standard
Karl–Fischer method and it was estimated to be below 30 ppm.
The structures of the bromide derivatives and of the ionic liquids
were identified by 1H and 13C NMR, FTIR and elemental
analysis. The results for BMMI and BMP salts are summarized
below. The BMITFSI data are not shown here due to extensive
literature data available [64–68]. It is important to note that the
yields obtained in both cases are lower than those reported by
Appetecchi et al. [69]. These differences could be assigned to
the use of bromide instead of iodine derivatives and also to the
loss of material during the purification processes.
BMMIBr data—mp 95–97 ◦C; found: C, 46.22; H, 6.96.
Calc for C9H17BrN2: C, 46.36; H, 7.35; νmax(KBr), cm−1:
3129, 3078, 2961, 2933, 2873, 1588, 1538, 1517, 1466, 1380,
1251 and 1136; δH (300 MHz, CDCl3, ppm): 0.97 (3H, t,
CH2CH2CH2CH3, J = 7 Hz), 1.40 (2H, m, CH2CH2CH2CH3),
1.81 (2H, m, CH2CH2CH2CH3), 2.83 (3H, s, CH3), 4.04 (3H,
s, NCH3), 4.25 (2H, t, CH2CH2CH2CH3, J = 7 Hz), 7.58 (1H,
d, CHring, J = 2.1 Hz) and 7.77 (1H, d, CHring, J = 2.1 Hz); δC
(75 MHz, CDCl3, ppm): 11.0, 13.6, 19.6, 31.8, 36.2, 48.8, 121.3,
123.1 and 143.7.
如果用软件翻译的麻烦别贴啦!
谢谢啦!
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