* 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.
Reference：
[1] Journal of the Chemical Society. Perkin Transactions 2, 1996, vol. 0, # 11, p. 2497 - 2504
[2] Journal of the Chemical Society. Perkin Transactions 2, 1996, vol. 0, # 11, p. 2497 - 2504
2
[ 100-22-1 ]
[ 100-22-1 ]
[ 153-18-4 ]
Reference：
[1] Journal of the Chemical Society. Perkin Transactions 2, 1996, vol. 0, # 11, p. 2497 - 2504
[2] Journal of the Chemical Society. Perkin Transactions 2, 1996, vol. 0, # 11, p. 2497 - 2504
3
[ 100-22-1 ]
[ 126216-42-0 ]
[ 100-22-1 ]
[ 56-69-9 ]
Reference：
[1] Journal of Physical Chemistry, 1982, vol. 86, p. 3661 - 3667
4
[ 100-22-1 ]
[ 548-83-4 ]
[ 100-22-1 ]
Reference：
[1] Journal of the Chemical Society. Perkin Transactions 2, 1996, vol. 0, # 11, p. 2497 - 2504
[2] Journal of the Chemical Society. Perkin Transactions 2, 1996, vol. 0, # 11, p. 2497 - 2504
poly(N,N'-bis[3-(dimethylamino)propyl]urea-co-1,4-dichlorobutane-co-N,N,N',N'-tetramethyl-1,4-phenylenediamine)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In ethanol; water; at 80 - 85℃; for 10.5h;Heating / reflux;
N,N'-Bis[3-(dimethylamino)propyl]urea (35 grams), N,N,N',N'-tetramethyl-1,4-phenylenediamine (15 grams), water (34 grams) and ethanol (47 grams) are introduced into a reaction flask equipped with a reflux condenser, thermometer and stirrer. The reagents are stirred and heated to reflux. 1,4-dichlorobutane (31 grams) is added slowly over 1.5 hours. The mixture is refluxed for 9 hours at 80-85° C. The resulting liquid is allowed to cool to room temperature giving an aqueous solution of the desired product.
(4-Dimethylamino-phenyl)-trimethyl-ammonium iodide (Compound 3) N,N,N',N'-Tetramethyl-benzene-1,4-diamine (200 mg, 1.22 mmol) was dissolved in dichloroethane (2 mL) and methyl iodide (173 mg, 1.22 mmol) was added dropwise. The reaction was refluxed for 1 hour, cooled to room temperature, the solid filtered out, washed with dichloromethane, dissolved in methanol and purified via flash column chromatography using a gradient of 0-8% MeOH:DCM to give 260 mg of grey solid (70% yield). 1H NMR (DMSO-d6): delta7.67 (d, J=9.3, 2H), 6.77 (d, J=9.3, 2H) 3.49 (s, 9H), 2.92 (s, 6H); MS (ESI, m/z): 179 (M+).
70%
In 1,2-dichloro-ethane; for 1.0h;Reflux;
N,N,N?,N?-Tetramethyl-benzene-1,4-diamine (200 mg, 1.22 mmol) was dissolved in dichloroethane (2 mL) and methyl iodide (173 mg, 1.22 mmol) was added dropwise. The reaction was refluxed for 1 hour, cooled to room temperature, the solid filtered out, washed with dichloromethane, dissolved in methanol and purified via flash column chromatography using a gradient of 0-8% MeOH:DCM to give 260 mg of grey solid (70% yield). 1H NMR (DMSO-d6): delta7.67 (d, J=9.3, 2H), 6.77 (d, J=9.3, 2H) 3.49 (s, 9H), 2.92 (s, 6H); MS (ESI, m/z): 179 (M+).
With sodium carbonate; In water; dimethyl sulfoxide; at 130℃; for 15.0h;Schlenk technique; Sealed tube; Green chemistry;
General procedure: In a typical procedure, a sealable Schlenk reaction tubeequipped with a magnetic stir bar was charged with the catalystCu/Al2O3 (6 mg, 27 mol% of Cu), p-nitrotoluene (0.25 mmol), paraformaldehyde(3.75 mmol), and Na2CO3 (0.5 mmol). Then, DMSOwater(3 mL, 1:1 v/v) was injected into the tube and the reactionwas tested under stirring at 130 C for 15 h. After completion ofthe reaction, the reaction mixture was extracted with ethyl acetateand then filtered. The liquid was analysed by GC and GC-MS on anAgilent HP-7890 instrument with a flame ionization detector (FID)and an HP-5MS capillary column (30 m, 0.25 mm i.d., 0.25 lm filmthicknesses) using nitrogen as the carrier gas to determine the conversionand selectivity using mesitylene as an internal standard.The desired N,N-dimethylated amines were purified by columnchromatography using an appropriate eluent and structurally confirmedby 1H/13C NMR and HR-MS.
With methanol; hydrogen; at 99.84℃; under 9750.98 Torr; for 1.83333h;Autoclave;
General procedure: The catalytic hydrogenation reaction was conducted in a stainless-steel autoclave reactor (70mL capacity) heated in oil bath. Substrate (6mmol), solvent (20mL) and catalyst (0.5g) were directly added into the reactor. The autoclave was purged with N2 and H2 three times before the reaction started. The reaction process was monitored by gas chromatography (GC) (Agilent 6890) with a flame ionization detector (FID) system.
4-(dimethylamino)phenyltrimethylammonium triflate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
45%
With K2[PtCl5CH3]; In dichloromethane; at 0℃; for 2.0h;Inert atmosphere;
General procedure: 165 mol of N,N-dialkylaniline was dissolved in 5mL dry dichloromethane. 5 mL of 33 mMmethyl trifluoromethanesulfonate (1 eq.) was added dropwise at 0 C over 3 minutes. Thereaction was stirred for 2h and the precipitate was filtered off, washed with dichloromethane anddried under vacuum.
[Tb2(O2CC6H3(NO2)2)6(DMSO)4] N,N,N',N'-tetramethyl-p-phenylenediamine 2acetonitrile[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
General procedure: KOH (79 mg, 1.41 mmol) was added with intense stirring to asolution of 3,5-dinitrobenzoic acid (300 mg, 1.41 mmol) in a mixtureof methanol (5 mL) and DMSO (1 mL). The mixture was stirredat room temperature for 20 min. Then a solution of LnCl36H2O(0.47 mmol) in a mixture of methanol (4 mL) and DMSO (1 mL)was added. The reaction mixture was stirred for 20-24 h. Thenthe reaction mixture was concentrated in vacuo using a water-jetpump to remove methanol. A hot (70 C) solution of TMPD(500 mg, 3.04 mmol) in 6 mL of CH3CN was added to the residue.The resulting dark violet solution was stirred for several minutes,filtered through a glass filter and allowed to cool slowly to roomtemperature on a water bath. The products (1-5a) precipitated in24 h as black crystals suitable for X-ray analysis. In cases of Yand Er, further cooling to 20 C was necessary to start crystallization.The products were washed with toluene and hexane, anddried in air. The yields were 55-65%.Compound 4b was obtained in a similar way, except that a solutionof 1600 mg (9.73 mmol) TMPD in 6 mL of CH3CN was used toextract the exchange product, and after the solution cooled toroom temperature, it was kept for two weeks at 20 C. The yieldwas 62%. According to X-ray diffraction analysis, in case of otherrare earth metals, except terbium and lighter-weight ones, mixturesof phases A and B formed under these conditions. In particular,a mixture of 90% 5a and 10% 5b was obtained in this way. Theuse of an extraction solution containing 2500 mg TMPD allowed amixture of 20% 5a and 80% 5b to be isolated in the case of yttrium;the product was isolated after keeping the solution for one monthat 20 C. These mixtures were used for EPR studies.Light colored crystals of complexes 6-12 were prepared similarlyusing pure CH3CN (6-7 mL) instead of the TMPD solutionfor extraction of the residue after removal of methanol from thereaction mixture. The color of 6-12 is determined by the cation.The yields were 45-50%.Complex 13. Similarly to the syntheses of 1-5a, the exchangereaction between potassium dinitrobenzoate and TbCl36H2O wascarried out in methanol in the presence of DMSO, then the solutionwas concentrated in vacuo. Subsequent extraction was performedusing a TMPD solution (1000 mg, 6.08 mmol) in 6 mL of CH3CN.Black crystals of complex 13 precipitated after keeping the extractat 20 C for one month. The yield was 20 mg (3.84%).
[Dy2(O2CC6H3(NO2)2)6(DMSO)4] N,N,N',N'-tetramethyl-p-phenylenediamine 2acetonitrile[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
General procedure: KOH (79 mg, 1.41 mmol) was added with intense stirring to asolution of 3,5-dinitrobenzoic acid (300 mg, 1.41 mmol) in a mixtureof methanol (5 mL) and DMSO (1 mL). The mixture was stirredat room temperature for 20 min. Then a solution of LnCl36H2O(0.47 mmol) in a mixture of methanol (4 mL) and DMSO (1 mL)was added. The reaction mixture was stirred for 20-24 h. Thenthe reaction mixture was concentrated in vacuo using a water-jetpump to remove methanol. A hot (70 C) solution of TMPD(500 mg, 3.04 mmol) in 6 mL of CH3CN was added to the residue.The resulting dark violet solution was stirred for several minutes,filtered through a glass filter and allowed to cool slowly to roomtemperature on a water bath. The products (1-5a) precipitated in24 h as black crystals suitable for X-ray analysis. In cases of Yand Er, further cooling to 20 C was necessary to start crystallization.The products were washed with toluene and hexane, anddried in air. The yields were 55-65%.Compound 4b was obtained in a similar way, except that a solutionof 1600 mg (9.73 mmol) TMPD in 6 mL of CH3CN was used toextract the exchange product, and after the solution cooled toroom temperature, it was kept for two weeks at 20 C. The yieldwas 62%. According to X-ray diffraction analysis, in case of otherrare earth metals, except terbium and lighter-weight ones, mixturesof phases A and B formed under these conditions. In particular,a mixture of 90% 5a and 10% 5b was obtained in this way. Theuse of an extraction solution containing 2500 mg TMPD allowed amixture of 20% 5a and 80% 5b to be isolated in the case of yttrium;the product was isolated after keeping the solution for one monthat 20 C. These mixtures were used for EPR studies.Light colored crystals of complexes 6-12 were prepared similarlyusing pure CH3CN (6-7 mL) instead of the TMPD solutionfor extraction of the residue after removal of methanol from thereaction mixture. The color of 6-12 is determined by the cation.The yields were 45-50%.Complex 13. Similarly to the syntheses of 1-5a, the exchangereaction between potassium dinitrobenzoate and TbCl36H2O wascarried out in methanol in the presence of DMSO, then the solutionwas concentrated in vacuo. Subsequent extraction was performedusing a TMPD solution (1000 mg, 6.08 mmol) in 6 mL of CH3CN.Black crystals of complex 13 precipitated after keeping the extractat 20 C for one month. The yield was 20 mg (3.84%).
[Ho2(O2CC6H3(NO2)2)6(DMSO)4] N,N,N',N'-tetramethyl-p-phenylenediamine 2acetonitrile[ No CAS ]
[Ho2(O2CC6H3(NO2)2)6(DMSO)4]3 N,N,N',N'-tetramethyl-p-phenylenediamine[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
General procedure: KOH (79 mg, 1.41 mmol) was added with intense stirring to asolution of 3,5-dinitrobenzoic acid (300 mg, 1.41 mmol) in a mixtureof methanol (5 mL) and DMSO (1 mL). The mixture was stirredat room temperature for 20 min. Then a solution of LnCl36H2O(0.47 mmol) in a mixture of methanol (4 mL) and DMSO (1 mL)was added. The reaction mixture was stirred for 20-24 h. Thenthe reaction mixture was concentrated in vacuo using a water-jetpump to remove methanol. A hot (70 C) solution of TMPD(500 mg, 3.04 mmol) in 6 mL of CH3CN was added to the residue.The resulting dark violet solution was stirred for several minutes,filtered through a glass filter and allowed to cool slowly to roomtemperature on a water bath. The products (1-5a) precipitated in24 h as black crystals suitable for X-ray analysis. In cases of Yand Er, further cooling to 20 C was necessary to start crystallization.The products were washed with toluene and hexane, anddried in air. The yields were 55-65%.Compound 4b was obtained in a similar way, except that a solutionof 1600 mg (9.73 mmol) TMPD in 6 mL of CH3CN was used toextract the exchange product, and after the solution cooled toroom temperature, it was kept for two weeks at 20 C. The yieldwas 62%. According to X-ray diffraction analysis, in case of otherrare earth metals, except terbium and lighter-weight ones, mixturesof phases A and B formed under these conditions. In particular,a mixture of 90% 5a and 10% 5b was obtained in this way. Theuse of an extraction solution containing 2500 mg TMPD allowed amixture of 20% 5a and 80% 5b to be isolated in the case of yttrium;the product was isolated after keeping the solution for one monthat 20 C. These mixtures were used for EPR studies.Light colored crystals of complexes 6-12 were prepared similarlyusing pure CH3CN (6-7 mL) instead of the TMPD solutionfor extraction of the residue after removal of methanol from thereaction mixture. The color of 6-12 is determined by the cation.The yields were 45-50%.Complex 13. Similarly to the syntheses of 1-5a, the exchangereaction between potassium dinitrobenzoate and TbCl36H2O wascarried out in methanol in the presence of DMSO, then the solutionwas concentrated in vacuo. Subsequent extraction was performedusing a TMPD solution (1000 mg, 6.08 mmol) in 6 mL of CH3CN.Black crystals of complex 13 precipitated after keeping the extractat 20 C for one month. The yield was 20 mg (3.84%).
[Er2(O2CC6H3(NO2)2)6(DMSO)4] N,N,N',N'-tetramethyl-p-phenylenediamine 2acetonitrile[ No CAS ]
[Er2(O2CC6H3(NO2)2)6(DMSO)4]3 N,N,N',N'-tetramethyl-p-phenylenediamine[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
62%
General procedure: KOH (79 mg, 1.41 mmol) was added with intense stirring to asolution of 3,5-dinitrobenzoic acid (300 mg, 1.41 mmol) in a mixtureof methanol (5 mL) and DMSO (1 mL). The mixture was stirredat room temperature for 20 min. Then a solution of LnCl36H2O(0.47 mmol) in a mixture of methanol (4 mL) and DMSO (1 mL)was added. The reaction mixture was stirred for 20-24 h. Thenthe reaction mixture was concentrated in vacuo using a water-jetpump to remove methanol. A hot (70 C) solution of TMPD(500 mg, 3.04 mmol) in 6 mL of CH3CN was added to the residue.The resulting dark violet solution was stirred for several minutes,filtered through a glass filter and allowed to cool slowly to roomtemperature on a water bath. The products (1-5a) precipitated in24 h as black crystals suitable for X-ray analysis. In cases of Yand Er, further cooling to 20 C was necessary to start crystallization.The products were washed with toluene and hexane, anddried in air. The yields were 55-65%.Compound 4b was obtained in a similar way, except that a solutionof 1600 mg (9.73 mmol) TMPD in 6 mL of CH3CN was used toextract the exchange product, and after the solution cooled toroom temperature, it was kept for two weeks at 20 C. The yieldwas 62%. According to X-ray diffraction analysis, in case of otherrare earth metals, except terbium and lighter-weight ones, mixturesof phases A and B formed under these conditions. In particular,a mixture of 90% 5a and 10% 5b was obtained in this way. Theuse of an extraction solution containing 2500 mg TMPD allowed amixture of 20% 5a and 80% 5b to be isolated in the case of yttrium;the product was isolated after keeping the solution for one monthat 20 C. These mixtures were used for EPR studies.Light colored crystals of complexes 6-12 were prepared similarlyusing pure CH3CN (6-7 mL) instead of the TMPD solutionfor extraction of the residue after removal of methanol from thereaction mixture. The color of 6-12 is determined by the cation.The yields were 45-50%.Complex 13. Similarly to the syntheses of 1-5a, the exchangereaction between potassium dinitrobenzoate and TbCl36H2O wascarried out in methanol in the presence of DMSO, then the solutionwas concentrated in vacuo. Subsequent extraction was performedusing a TMPD solution (1000 mg, 6.08 mmol) in 6 mL of CH3CN.Black crystals of complex 13 precipitated after keeping the extractat 20 C for one month. The yield was 20 mg (3.84%).
[Y2(O2CC6H3(NO2)2)6(DMSO)4] N,N,N',N'-tetramethyl-p-phenylenediamine 2acetonitrile[ No CAS ]
[Y2(O2CC6H3(NO2)2)6(DMSO)4]3 N,N,N',N'-tetramethyl-p-phenylenediamine[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
90%; 10%
General procedure: KOH (79 mg, 1.41 mmol) was added with intense stirring to asolution of 3,5-dinitrobenzoic acid (300 mg, 1.41 mmol) in a mixtureof methanol (5 mL) and DMSO (1 mL). The mixture was stirredat room temperature for 20 min. Then a solution of LnCl36H2O(0.47 mmol) in a mixture of methanol (4 mL) and DMSO (1 mL)was added. The reaction mixture was stirred for 20-24 h. Thenthe reaction mixture was concentrated in vacuo using a water-jetpump to remove methanol. A hot (70 C) solution of TMPD(500 mg, 3.04 mmol) in 6 mL of CH3CN was added to the residue.The resulting dark violet solution was stirred for several minutes,filtered through a glass filter and allowed to cool slowly to roomtemperature on a water bath. The products (1-5a) precipitated in24 h as black crystals suitable for X-ray analysis. In cases of Yand Er, further cooling to 20 C was necessary to start crystallization.The products were washed with toluene and hexane, anddried in air. The yields were 55-65%.Compound 4b was obtained in a similar way, except that a solutionof 1600 mg (9.73 mmol) TMPD in 6 mL of CH3CN was used toextract the exchange product, and after the solution cooled toroom temperature, it was kept for two weeks at 20 C. The yieldwas 62%. According to X-ray diffraction analysis, in case of otherrare earth metals, except terbium and lighter-weight ones, mixturesof phases A and B formed under these conditions. In particular,a mixture of 90% 5a and 10% 5b was obtained in this way. Theuse of an extraction solution containing 2500 mg TMPD allowed amixture of 20% 5a and 80% 5b to be isolated in the case of yttrium;the product was isolated after keeping the solution for one monthat 20 C. These mixtures were used for EPR studies.Light colored crystals of complexes 6-12 were prepared similarlyusing pure CH3CN (6-7 mL) instead of the TMPD solutionfor extraction of the residue after removal of methanol from thereaction mixture. The color of 6-12 is determined by the cation.The yields were 45-50%.Complex 13. Similarly to the syntheses of 1-5a, the exchangereaction between potassium dinitrobenzoate and TbCl36H2O wascarried out in methanol in the presence of DMSO, then the solutionwas concentrated in vacuo. Subsequent extraction was performedusing a TMPD solution (1000 mg, 6.08 mmol) in 6 mL of CH3CN.Black crystals of complex 13 precipitated after keeping the extractat 20 C for one month. The yield was 20 mg (3.84%).
20%; 80%
General procedure: KOH (79 mg, 1.41 mmol) was added with intense stirring to asolution of 3,5-dinitrobenzoic acid (300 mg, 1.41 mmol) in a mixtureof methanol (5 mL) and DMSO (1 mL). The mixture was stirredat room temperature for 20 min. Then a solution of LnCl36H2O(0.47 mmol) in a mixture of methanol (4 mL) and DMSO (1 mL)was added. The reaction mixture was stirred for 20-24 h. Thenthe reaction mixture was concentrated in vacuo using a water-jetpump to remove methanol. A hot (70 C) solution of TMPD(500 mg, 3.04 mmol) in 6 mL of CH3CN was added to the residue.The resulting dark violet solution was stirred for several minutes,filtered through a glass filter and allowed to cool slowly to roomtemperature on a water bath. The products (1-5a) precipitated in24 h as black crystals suitable for X-ray analysis. In cases of Yand Er, further cooling to 20 C was necessary to start crystallization.The products were washed with toluene and hexane, anddried in air. The yields were 55-65%.Compound 4b was obtained in a similar way, except that a solutionof 1600 mg (9.73 mmol) TMPD in 6 mL of CH3CN was used toextract the exchange product, and after the solution cooled toroom temperature, it was kept for two weeks at 20 C. The yieldwas 62%. According to X-ray diffraction analysis, in case of otherrare earth metals, except terbium and lighter-weight ones, mixturesof phases A and B formed under these conditions. In particular,a mixture of 90% 5a and 10% 5b was obtained in this way. Theuse of an extraction solution containing 2500 mg TMPD allowed amixture of 20% 5a and 80% 5b to be isolated in the case of yttrium;the product was isolated after keeping the solution for one monthat 20 C. These mixtures were used for EPR studies.Light colored crystals of complexes 6-12 were prepared similarlyusing pure CH3CN (6-7 mL) instead of the TMPD solutionfor extraction of the residue after removal of methanol from thereaction mixture. The color of 6-12 is determined by the cation.The yields were 45-50%.Complex 13. Similarly to the syntheses of 1-5a, the exchangereaction between potassium dinitrobenzoate and TbCl36H2O wascarried out in methanol in the presence of DMSO, then the solutionwas concentrated in vacuo. Subsequent extraction was performedusing a TMPD solution (1000 mg, 6.08 mmol) in 6 mL of CH3CN.Black crystals of complex 13 precipitated after keeping the extractat 20 C for one month. The yield was 20 mg (3.84%).
[Tb(O2CC6H3(NO2)2)3(DMSO)(H2O)]n0.5nN,N,N',N'-tetramethyl-p-phenylenediamine 1.5nDMSO0.5nacetonitrile[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
3.84%
General procedure: KOH (79 mg, 1.41 mmol) was added with intense stirring to asolution of 3,5-dinitrobenzoic acid (300 mg, 1.41 mmol) in a mixtureof methanol (5 mL) and DMSO (1 mL). The mixture was stirredat room temperature for 20 min. Then a solution of LnCl36H2O(0.47 mmol) in a mixture of methanol (4 mL) and DMSO (1 mL)was added. The reaction mixture was stirred for 20-24 h. Thenthe reaction mixture was concentrated in vacuo using a water-jetpump to remove methanol. A hot (70 C) solution of TMPD(500 mg, 3.04 mmol) in 6 mL of CH3CN was added to the residue.The resulting dark violet solution was stirred for several minutes,filtered through a glass filter and allowed to cool slowly to roomtemperature on a water bath. The products (1-5a) precipitated in24 h as black crystals suitable for X-ray analysis. In cases of Yand Er, further cooling to 20 C was necessary to start crystallization.The products were washed with toluene and hexane, anddried in air. The yields were 55-65%.Compound 4b was obtained in a similar way, except that a solutionof 1600 mg (9.73 mmol) TMPD in 6 mL of CH3CN was used toextract the exchange product, and after the solution cooled toroom temperature, it was kept for two weeks at 20 C. The yieldwas 62%. According to X-ray diffraction analysis, in case of otherrare earth metals, except terbium and lighter-weight ones, mixturesof phases A and B formed under these conditions. In particular,a mixture of 90% 5a and 10% 5b was obtained in this way. Theuse of an extraction solution containing 2500 mg TMPD allowed amixture of 20% 5a and 80% 5b to be isolated in the case of yttrium;the product was isolated after keeping the solution for one monthat 20 C. These mixtures were used for EPR studies.Light colored crystals of complexes 6-12 were prepared similarlyusing pure CH3CN (6-7 mL) instead of the TMPD solutionfor extraction of the residue after removal of methanol from thereaction mixture. The color of 6-12 is determined by the cation.The yields were 45-50%.Complex 13. Similarly to the syntheses of 1-5a, the exchangereaction between potassium dinitrobenzoate and TbCl36H2O wascarried out in methanol in the presence of DMSO, then the solutionwas concentrated in vacuo. Subsequent extraction was performedusing a TMPD solution (1000 mg, 6.08 mmol) in 6 mL of CH3CN.Black crystals of complex 13 precipitated after keeping the extractat 20 C for one month. The yield was 20 mg (3.84%).
[11C]-(4-dimethylaminophenyl)trimethylammonium iodide[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In acetonitrile; at -15 - 80℃;
11C]MeI was produced as described for [11C]-1 and distilled to the second reactor, containing N,N,N?,N?-tetramethyl-benzene-1,4-diamine (20 mg, 0.12 mmol) and 280 muL of acetonitrile. After 1 min of distillation, an average of 500±60 mCi (n=4) was trapped in the second reactor at -15 C. The reactor was sealed and heated to 80 C. for 5 minutes. At the end of the 5 minute reaction, the reaction temperature was raised to 100 C. under vacuum for one minute in order to evaporate volatiles. The crude product was diluted with water (2 mL) and automatically injected to the HPLC (system C), rt=13 minutes. The labeled product (150±31 mCi) was collected in a flask and a sample was diluted with saline to give a final solution of the tracer in 1:9 EtOH:phosphate buffer (pH 5.5). Radiochemical yield was 52%±11 decay corrected to EOB with a total synthesis time of 40 min, specific activity of 3.3±0.5 Ci/mumole and radiochemical purity higher than 99%.
Into a synthetic kettle equipped with a reflux condenserN, N, N ', N'-tetramethyl-p-phenylenediamineSolution,Starting the stirrer, 2.2 times the molar amount of epichlorohydrin at 70 C,Slowly dropping synthetic kettle, after dripping, continue to respond for 12h, stop the reaction.The mixture of the resulting solution product is then carefully distilled or solvent extracted to remove the remainingReaction compounds and by-products, the control system temperature is about 30 , the pressure in the 1-4kPa. Collect volatility with a dry ice collectorMaterial until the product solution is concentrated to a thick slurry. The resulting thick slurry is a double reactivity dicarboxylic acid groupCationic modifier, as shown in Formula I-3
In [(2)H6]acetone; water-d2; at 22℃; for 2.0h;Inert atmosphere;Kinetics;
General procedure: 165 mol of N,N-dialkylaniline was dissolved in 5mL dry dichloromethane. 5 mL of 33 mMmethyl trifluoromethanesulfonate (1 eq.) was added dropwise at 0 C over 3 minutes. Thereaction was stirred for 2h and the precipitate was filtered off, washed with dichloromethane anddried under vacuum.
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