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[ CAS No. 103595-81-9 ]

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Chemical Structure| 103595-81-9
Chemical Structure| 103595-81-9
Structure of 103595-81-9 *Storage: {[proInfo.prStorage]}
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Product Details of [ 103595-81-9 ]

CAS No. :103595-81-9MDL No. :N/A
Formula : C32H48N2O2 Boiling Point : -
Linear Structure Formula :-InChI Key :N/A
M.W :492.74Pubchem ID :-
Synonyms :

Computed Properties of [ 103595-81-9 ]

TPSA : - H-Bond Acceptor Count : -
XLogP3 : - H-Bond Donor Count : -
SP3 : - Rotatable Bond Count : -

Safety of [ 103595-81-9 ]

Signal Word:WarningClass:
Precautionary Statements:P261-P280-P301+P312-P302+P352-P305+P351+P338UN#:
Hazard Statements:H302-H315-H319-H335Packing Group:
GHS Pictogram:

Application In Synthesis of [ 103595-81-9 ]

  • Downstream synthetic route of [ 103595-81-9 ]

[ 103595-81-9 ] Synthesis Path-Downstream   1~10

  • 1
  • [ 37942-07-7 ]
  • [ 107-15-3 ]
  • N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-ethylenediamine [ No CAS ]
YieldReaction ConditionsOperation in experiment
72% In methanol;Reflux; General procedure: The Schiff bases used for the synthesis of the catalysts were prepared by the well known reaction between salicylaldehyde and diamine. Slight experimental variations were introduced with respect to literature methods [27] and the resulting procedure was successfully applied to a number of differently substituted aldehydes. (0015) General procedure: Two equivalents of the appropriate salicylaldehyde were dissolved in the minimum volume of boiling methanol (generally, 20 ml) and added dropwise with one equivalent of diamine (either 1,2-diaminoethane or 1,2-benzenediamine) in 5 ml methanol. The solution was refluxed until all the aldehyde disappeared (TLC analysis) and then cooled to room temperature, thus causing precipitation of the Schiff base, as a yellow solid. The filtered solid was washed with a small amount of methanol, then with diethyl ether and dried. The following Schiff bases were prepared: (0016) Salophen, [1,2-bis-(salicylideneamino)benzene]: yield 95.3%; 5,5′-Cl2salophen, [1,2-bis-(5-Cl-salicylideneamino)benzene]: yield >99%; 5,5′-(t-Bu)2salophen [1,2-bis-(5-t-Bu-salicylideneamino)benzene]: yield 75%; 3,3′-(OMe)2salophen, [1,2-bis-(3-OMe-salicylideneamino)-benzene]: yield 77%; 5,5′-(OMe)2salophen, [1,2-bis-(5-OMe-salicylideneamino)-benzene]: yield 79%; 3,3′,5,5′-Cl4salophen [1,2-bis-(3,5-Cl2salicylideneamino)benzene]: yield 95%; 3,3′,5,5′-(t-Bu)4salophen [1,2-bis-(3,5-di-t-Bu-salicylideneamino)benzene]: yield 75%. (0017) Salen, [1,2-bis-(salicylideneamino)ethane]: yield 88%; 5,5′-Cl2salen, [1,2-bis-(5-Cl-salicylideneamino)ethane]: yield 67%; 5,5′-(t-Bu)2salen, [1,2-bis-(5-t-Bu-salicylideneamino)ethane]: yield 91%; 3,3′-(OMe)2salen, [1,2-bis-(3-methoxy-salicylideneamino)ethane]: yield 92%; 5,5′-(OMe)2salen, [1,2-bis-(5-OMe-salicylideneamino)ethane]: yield 92%; 3,3′,5,5′-Cl4salen, [1,2-bis-(3,5-Cl2-salicylideneamino)ethane]: yield 70%; 3,3′,5,5′-(t-Bu)4salen, [1,2-bis-(3,5-(t-Bu)2-salicylideneamino)ethane]: yield 72%. (0018) All the compounds gave 1H NMR and UV-vis spectra consistent with the structure and with literature data [25,28-30].
In methanol;Reflux; General procedure: Two equivalents of the appropriate salicylaldehyde were dissolved in the minimum volume of boiling methanol and one equivalent of 1,2-diaminoethane in 5 mL methanol was added dropwise. The solution was refluxed until all the aldehyde disappeared and then cooled to room temperature, thus causing precipitation of the Schiff base as a yellow solid. The filtered solid was washed with a small amount of methanol, then with diethyl ether and dried.
In ethanol; General procedure: Schiff base ligands and their corresponding complexes [NN-bis-(3,5-di-tert-butylsalicylidene)-ethylendiamine]manganese(III)chloride [Mn(3,5-dtSALEN)Cl)] (I) and [NN-bis-(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediamine]manganese(III)chloride [Mn(3,5-dtSALHD)Cl] (II) were prepared adopting amethodology widely reported in the literature [13,19,38-40].The ligands were prepared by condensation of 3,5-di-tert-butylsalicylaldehyde with the corresponding diamine (either,ethylenediamine or 1,2-cyclohexanediamine) in a molar ratio 1:2in ethanol. Complexes (I) and (II) were obtained then by addinga saturated solution prepared with 3.66 mmol of manganeseacetate in absolute ethanol to 1.83 mmol of the correspondingligand dissolved in 25 cm3of the same solvent pre-heated at353 K under reflux; air was slowly and shortly (10-20 s) bubbledthrough the reacting mixture since long oxidation might leadto form oxo-Mn(V) species easily detected by darkening of thebrownish solution [41], which inactivate the catalytic responseof the complexes in the targeted reaction. Then, the air streamwas stopped and the heating was kept along one extra hour withdarkening of the yellow-orange solution to brown. Afterwards,5.29 mmol of lithium chloride in ethanol were added to achieve theaccess of Cl into the coordination sphere of the transition metal,and the mixture was heated further 30 min. The resulting solidwas then dissolved in dichloromethane and refined employingthe method from Cubillos et al. [40] by means of liquid extractionwith n-heptane. The final solid was recovered by vacuum filtering and filteringand then dried at room temperature in a desiccator. The sameprocedure was used to prepare both complexes
In ethanol; at 80℃; for 12h; 0.6 g of 1, 2-ethanediamine is dissolved in 20mL of ethanol, obtained 1, 2-ethanediamine solution; 4.7 g of 3,5-di-tert-butyl salicylaldehyde is dissolved in 30mL of ethanol, obtained 3,5-di-tert-butyl salicylaldehyde solution, 3,5-di-tert-butyl salicylaldehyde is slowly added drop-wise to the 1,2-ethanediamine solution, the obtained mixed solution is refluxed at 80 C for 12 h, and then obtained reaction mixture. The solvent in the reaction mixture is removed by filtration; the resulting reaction product is re-crystallized from ethanol and then obtained Schiff base ligand. In the present invention, the obtained Schiff base compound is subjected to elemental analysis, and obtained the content of each atom, the results are as follows: Elem.Anal. (%):Calcd.C 78.00, H9.82, N 5.69; Found C 77 · 58, Η 9.88, N 5.77. This means, The Schiff base ligand which is obtained in this example has the structure represented by the formula (II), among them, Y for 1, 2-ethyl; R for Tert-butyl.
10.12 g In ethanol;Reflux; General procedure: For the synthesis of L1, 1.4 mL ethylenediamine(20mmol) was added to a solution of 4.5mL salicylaldehyde(41mmol) with 50mL ethanol in a round bottomflask. The reaction mixture was thoroughly stirredat refluxing temperature for 3-4h, or until flaky yellowcrystals were formed, and the solution was then left to coolin an ice-bath. The crystals were fltered and washed, thenair-dried. Yield of L1 was found to be 5.2g. For the synthesisof L2, 7.31g 3-tert-butyl-2-hydroxybenzaldehyde;and for L3, 9.6g 3,5-di-tert-butyl-2-hydroxybenzaldehydewas taken in place of salicylaldehyde. The yield of L2 andL3 were obtained 8.23g and 10.12g, respectively.

  • 2
  • N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-ethylenediamine [ No CAS ]
  • [ 98-80-6 ]
  • C44H56B2N2O3 [ No CAS ]
  • 3
  • [ 20398-06-5 ]
  • N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-ethylenediamine [ No CAS ]
  • [((μ-O)2,κ1—(N)(N′)salo-But)Tl2] [ No CAS ]
YieldReaction ConditionsOperation in experiment
In toluene; for 12h; The present invention is directed to the synthesis and characterization of thallium salen fluorescent tracers. The general reaction for these compounds is shown in eq 1. <in-line-formulae>2[Tl(OR*)]+H2-saloR′-R→[Tl2(saloR′-R)]+2HOR*(1)</in-line-formulae> where Tl(OR*) is a thallium alkoxide and H2-saloR′-R is a salen ligand. R is a substituent on the salen ring and can be a wide variety of functional groups, including, but not limited to, hydrocarbons, nitrates, sulfates, alkoxides (methoxide), etc. R′ is the linkage in the salen and can be an alkyl, phenyl, cyclohexyl, or hydrogen, for example. (0019) As examples of the invention, the coordination behavior of Tl(I) with two salen ligands is described below. These exemplary thallium salens were synthesized according to the reaction: <in-line-formulae>2[Tl(OEt)]+H2-saloR′-But→[Tl2(saloR′-But)]+2HOEt(2)</in-line-formulae> (0020) where R′=CH2CH2 or C6H4. For these reactions, thallium ethoxide [Tl(OEt)] was reacted with N,N′-bis(3,5-di-t-butylsalicylidene)-ethylenediamine (H2-salo-But) or N,N′-bis(3,5-di-t-butylsalicylidene)-1,2-phenylenediamine (H2-saloPh-But). The products were identified by single crystal X-ray diffraction as: [((μ-O)2,κ1-(N)(N′)salo-But)Tl2], hereinafter referred to as compound 1, and {[((μ-O)2saloPh-But)Tl2][[((μ-O)2,κ1-(N)(N′)saloPh-But)Tl2]}, hereinafter referred to as compound 2. FIG. 1(a) shows a schematic representation of the synthesis of compound 1. FIG. 1(b) shows a schematic representation of the synthesis of compound 2. (0021) The synthesis of the exemplary Tl-salen compounds began with a 1:1 stoichiometry of [Tl(OEt)] and the appropriate H2-saloR′-But. H2-salo-But or H2-saloPh-But were synthesized from the reaction of ethylenediamine with either 3,5-di-tert-butyl-2-hydroxybenzaldehyde or ortho-phenylenediamine, respectively. See C. Sohn et al., Dalton Trans. 45, 5825 (2016). Each precursor was individually dissolved in toluene and then the colorless Tl solution was slowly added to the bright yellow H2-saloR′-But solutions. The Tl/salo-But reaction turned to a bright orange color, whereas the Tl/saloPh-But mixture turned to a cherry red color. After stirring for 12 h, the cap was removed to allow for the volatile component to evaporate. X-ray quality crystals were isolated by slow evaporation and solved as the [Tl2(saloR′-But)] complexes 1 and 2. A rational synthesis was undertaken using a 2:1 [Tl(OEt)]:H2-saloR′-But ratio. The same products were isolated but lacked the residual H2-saloR′-But impurity associated with the original 1:1 stoichiometry. Therefore, the following experimental data are for the rational synthesis 2:1 stoichiometry route.
  • 4
  • [ 109-63-7 ]
  • N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-ethylenediamine [ No CAS ]
  • C32H46B2F4N2O2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
With N-ethyl-N,N-diisopropylamine; In toluene; at 40℃; for 2.5h;Inert atmosphere; Under a nitrogen atmosphere,15.0 g (30 mmol) of N, N'-bis (3,5-di-tert-butylsalicylidene) -1,2 ethylenediamine,Boron trifluoride-ether complex21.6g (152mmol), 300ml toluene,20 g (152 mmol) of N, N-diisopropylethylamine was stirred with heating at 40 C for 2.5 hours.Cool to room temperature, add 300ml of water, and separate the filtrate into organic and aqueous layers.The organic layer was washed twice with a saturated sodium carbonate aqueous solution and dried over magnesium sulfate.The obtained solid was recrystallized from toluene (150 ml) and ethanol (750 ml),This gave 17.89 g of crude product.The crude product is under pressure 3 × 10-3Pa,Sublimation at a temperature of 220 C gave compound [51] (light yellow solid).
  • 5
  • (3,5)-di-tert butylsalicylaldehyde [ No CAS ]
  • [ 107-15-3 ]
  • N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-ethylenediamine [ No CAS ]
  • 6
  • iron(III) chloride [ No CAS ]
  • N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-ethylenediamine [ No CAS ]
  • C32H46ClFeN2O2 [ No CAS ]
  • 7
  • [ 110-86-1 ]
  • N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-ethylenediamine [ No CAS ]
  • [(κ4-(O,N,N′,O′)salo-But)Ca(pyridine)3] [ No CAS ]
  • 8
  • [ 110-86-1 ]
  • N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-ethylenediamine [ No CAS ]
  • [(κ4-(O,N,N′,O′)salo-But)Mg(pyridine)2] [ No CAS ]
  • 9
  • [ 122-51-0 ]
  • N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-ethylenediamine [ No CAS ]
  • 1,3-bis(3,5-di-tert-butyl-2-hydroxybenzyl)-4,5-dihydro-1H-imidazolinium chloride [ No CAS ]
  • 10
  • [ 75-24-1 ]
  • N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-ethylenediamine [ No CAS ]
  • C36H58Al2N2O2 [ No CAS ]
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