After filtration of reaction mixture, a solid material was obtained and was dried in vacuum to obtain colorless crystalline solid. Spirocyclic compounds C 35a — C 35c were synthesized by adding n-butyl lithium in n-hexane into a solution of 2- phenylaminomethyl phenol in diethyl ether Scheme After filtration, the reaction mixture was washed with n-pentane and was then dried under low pressure. The solid was dispersed in toluene and GeCl 4 was added dropwise with the help of syringe. The solution was filtered using celite and was concentrated in vacuum and hence finally gave solids, which were crystallized from an appropriate solvent.
All volatiles were removed using rotary evaporator. The orange crude product was extracted with toluene, and the solution was filtered through celite The filtered material was evaporated to obtain a solid. All volatiles were removed under low pressure. The residue was extracted three times by pentane. The white solid was washed with cold n-pentane, and the product was dried in vacuum.
After removing solvent from reaction mixture, the solid residue was dissolved in n-pentane. A white crystalline solid was extracted out from solution and was washed with clean and cold n-pentane. The extracted product was dried in vacuum. THF 2 in toluene at room temperature. The extracted residue was washed several times by n-pentane and was dried under vacuum.
C 40 was synthesized in two steps Scheme The reaction mixture was stirred continuously at room temperature overnight. The reaction mixture was filtered to remove sodium chloride salt as by-product. After filtration, the filtrate was concentrated in vacuum to obtain Ge dmamp 2 as crude product. Sulfur powder was then added slowly into a solution of Ge dmamp 2 in toluene.
Modern synthesis (20th century)
The reaction mixture was stirred at room temperature overnight. C 40 was obtained as a white solid after removing all the volatiles from the reaction mixture. C 42 was formed when elemental sulfur was added into L 28 solution in THF at room temperature. All volatiles were removed under reduced pressure.
Single crystals of C 42 were obtained by the slow evaporation of solvent from its chloroform solution. Crystals of C 42 were remained suitable for X-ray crystallographic studies. After mixing, immediately a milky solid suspension was observed.
The reaction mixture was then cooled and N,N-di-tert-butylchloro phenylamidinate -germanium II was added dropwise in the reaction mixture. After complete addition, the reaction mixture was maintained at ambient temperature overnight. All volatile solvents were removed in vacuum.
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C 43 was extracted with the addition of hot hexane in reaction mixture via cannula filtration. After filtration, the filtrate was placed in Schlenk tube and the tube was taken outside the glove box. The residue was filtered through syringe filter in a glove box by using Et 2 O. The resulting residue was redissolved in pentane and was concentrated to remove uncoordinated THF. C 45 was synthesized when iodine was added to a solution of L 32 Scheme Yellow solid product was washed with toluene and was dried in vacuum.
Single crystals of C 46 were grown from its hot acetonitrile solution for X-ray diffraction studies. The yellow solid was washed with n-hexane and was dried in vacuum to obtain pure sample of C 47 as yellow solid. L 34 in CH 3 CN was placed in a round bottom flask under an inert atmosphere using argon gas Scheme Triethyleneamine NEt 3 and GeCl 4 were added in the reaction medium. All volatiles were removed. C 49 was formed when elemental sulfur was added into a solution of L 35 in THF at room temperature Scheme The residue was washed with n-hexane and dried to obtain product as yellow solid.
Single crystals of complex were obtained by evaporation method. According to this method, a slow evaporation of solvent from its saturated solution in chloroform was managed to obtain crystals suitable for X-ray diffraction study. C 50 was obtained when selenium powder was added slowly into a Ge dmampS 2 solution in toluene Scheme All volatiles were removed from reaction mixture under vacuum.
The Synthesis and Spectral Analysis of Au(III) Complex of Caffeine and Nicotinamide
The product was obtained as yellow solid. The pure product was synthesized by recrystallization of yellow solid from an ether solution. The product was extracted twice with n-pentane. C 52 was formed when a solution of L 38 was added dropwise to a stirred suspension of Mn 2 CO 10 in toluene at room temperature Scheme The reaction mixture was refluxed overnight. After filtration, the filtrate was concentrated. The end product was obtained as dark red crystals in C 53 was formed when N-methoxypropanamide was added dropwise to a stirring diethyl ether solution of L 39 Scheme L 40 was dissolved in THF and n-butyl lithium was added into reaction mixture through a syringe Scheme GeCl 2 was added as a solid, and dark yellow solution was formed.
C 55 was synthesized when superhydride was added into the solution of naphthol in THF Scheme CH 3 2 GeCl 2 was added and the reaction mixture was stirred overnight. The product was dissolved in DCM and filtered through celite. The product was washed with hexane. All volatiles were removed under vacuum and were extracted with toluene.
Zeitschrift für Kristallographie - New Crystal Structures
At that time, the reaction flask was wrapped with aluminum foil to protect day light. The precipitate of NaCl was separated from reaction mixture through centrifugation. Then, the residue was washed with n-hexane and extracted with diethyl ether. The color of reaction mixture changed immediately into pale yellow. After addition of n-hexane in flask, the reaction mixture was cooled slowly.
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Phillips, B. Patrick and W.