Ethyl 3,5-dinitrobenzoate

Heat together under very efficient water reflux 1 g. of freshly fused dry powdered ZnClg, 2 ml. of diethyl ether and 0 5 g. of 3,5 -dinitrobenzoyl chloride for 2 hours. Shake the product with 5 ml. of water and ther add 10% NaOH solution until all the ZnCl, and excess of 3,5-dinitro> benzoyl chloride and 3,5-dinitrobenzoic acid have gone into solution. Filter at the pump and recrystallise from petroleum (b.p. 40-60°) to obtain ethyl 3,5-dinitrobenzoate, m.p. 93°. (M ps. of other 3,5 dinitro-benzoates, p. 536.)... 

Ethyl 3,5-dinitrobenzoate Methyl 3,5-dinitrobenzoate Ethyl 2,4-dinitrobenzoate Methyl 2,4-dinitrobenzoate... 

Ethyl-3,5-dinitrobenzoate, ndls (from ale), sp gr 1.295 at 111°, mp 91—2°, bp — not given insol in w si sol in ale. It may be prepd from the silver salt of the acid and ethyl iodide, from the acid and ale HC1 . from the acid chloride in benzene from the chloride and ether with zinc chloride... 

J. Houben obtained methane, etc., by the action of magnesium alkyl haloids on the hydrazines the action of zinc ethyl and magnesium alkyl haloids on hydrazine has been studied by R. L. Krause the action of mono- and di- chloroacetic acids, by Jit. Busch and E. Meussdorffer ethyl chloroacetate, by A. Reissert and W. Kayser, and M. Busch and eo-workers phenylglyoxalic acid, by A. Elbers dinitrophenylhydrazine, by T. Curtius and M. Mayer ethyl dinitrobenzoate, by T. Curtius and A. Riedel dinitrobenzoic add, by T. Curtius and H. E. Bollenbach nitro- and amido-phthalhydrazides, by T. Curtius and A. Hoesch formaldehyde, by E. Riegler, and E. Rimini carbonyl compounds, by... 

Dinitrobenzoate light yellow crysts, mp 121.8° prepd by the interaction of the components in hot abs ethyl ale. It is also used to isolate and identify N-methylaniline... 

For example, oily ( + )-ethyl (7 )-4,4,4-trifluoro-3-hydroxybutanoate (2) is obtained with 45% cc from ethyl 4.4,4-trifluoro-3-oxobutanoate (1). The 3,5-dinitrobenzoate of 2 shows the phase diagram of a racemic compound with an eutectic composition of 35 15. This allows the isolation of a limited quantity of the pure crystalline enantiomer, which is then reconverted into 2 by transesterification in ethanol13. 

Ethyl 4mamino-3t5 dinitrobenzoate gold-glimmering leaflets, mp 114°. It may be prepd by esterification of die acid in ale HC1 Ref Beil 14, 458... 

Ethy1-2,6-dinitrobenzoate, crysts (from ale), rap 74.7°. It may be prepd from the silver salt of the acid and ethyl iodide Ref Beil. 9, 413... 

Ethyl p-aminobenzoate and derivs 6 E203 ethyl p-amino-dinitrobenzoates 6 E203 ethyl p-aminonitrobenzoates 6 E203... 

Dinitrobenzamide, lfts(from w), mp 177-183° diffc sol in cold w, more readily sol in hot w prepd by reacting 3,5-dinitrobenzoic acid ethyl ester or 3,5-dinitrobenzoyl chloride with NH3(Ref2) Refs l)Beil9,412 2)Beil9,414 2,4,6 Trinitrobenzamide,(02N)3C6H2.CO.NH2 ... 

N 24.78%. Two isomers are described in the literature 2,4-Dinitrobenzoic Acid Hydrazide (2,4 -Dinitrobenzoic Acid Hydrazide), orn-yel cryst (from abs ale), mp 231-3° was prepd in small quant by treating the methyl or ethyl ester of 2,4 -dinitrobenzoic acid with hydrazine sulfare(Ref 3)... 

Dinitrobenzoic Acid Hydrazide(called 3.5-Di-nitro-benzoylhydrazid in Ger), yel ndls(from ale), mp 158° was prepd by heating the ethyl ester of... 

Rate and equilibrium constants have been reported for the reactions of butylamine, pyrrolidine, and piperidine with trinitrobenzene, ethyl 2,4,6-trinitrophenyl ether, and phenyl 2,4,6-trinitrophenyl ether in acetonitrile, hi these reactions, leading to cr-adduct formation and/or nucleophilic substitution, proton transfer may be rate limiting. Comparisons with data obtained in DMSO show that, while equilibrium constants for adduct formation are lower in acetonitrile, rate constants for proton transfer are higher. This probably reflects the stronger hydrogen bonding between DMSO and NH+ protons in ammonium ions and in zwitterions.113 Reaction of 1,3,5-trinitrobenzene with indole-3-carboxylate ions in methanol has been shown to yield the re-complex (26), which is the likely precursor of nitrogen- and carbon-bonded cr-adducts expected from the reaction.114 There is evidence for the intermediacy of adducts similar to (27) from the reaction of methyl 3,5-dinitrobenzoate with l,8-diazabicyclo[5.4.0]undec-8-ene (DBU) cyclization eventually yields 2-aminoindole derivatives.115... 

A N-Dimethylglycine (0) 3,5-Dinitrobenzoic acid (0) 2-Ethylbutyric acid (0) 5-Ethyl-5-phenylbarbituric acid (0) Fluoroacetic acid (0)... 

Bromo-2,7-dinitrobenzo / thiophene-5-diazonium-4-oxide, 2878a f 2-Bromoethyl ethyl ether, 1630... 

Hydroxy-3-butenonitrile, see l-Cyano-2-propen-l-ol, 1463 4-Hydroxy-fraws-cinnamic acid, 3130 Hydroxycopper(II) glyoximate, 0795 4-Hydroxy-3,5 -dimethyl-1,2,4-triazole, 1570 4-Hydroxy-3,5-dinitrobenzenearsonic acid, 2213 2-Hydroxy-3,5-dinitrobenzoic acid, see 3,5-Dinitrosalicylic acid, 2661 2-Hydroxy-3,5-dinitropyridine, 1816 N-Hydroxydithiocarbamic acid, 0453 2(2-Hydroxyethoxy)ethyl perchlorate, 1638 (9-(2-Hydroxyethyl)hydroxylamine, 0940... 

Preparaton of the Enantiomers of Ethyl 3-Hydroxybutanoate. Reduction of ethyl acetoacetate with yeast yields ethyl (S)-3-hydroxybutanoate (15) as shown in Figure 4 (12-14). Purification of crude 15 as its crystalline 3,5-dinitrobenzoate gives (S)-15 of 100% e.e. (14,15). 

The mixture is allowed to cool and is poured into 800 g. of ice and.800 cc. of water. After standing for thirty minutes the 3,5-dinitrobenzoic acid is filtered with suction and washed with water until free of sulfates. The crude product weighs 62-65 g. and melts at 200-202°. This product is recrystallized from 275 cc. of hot 50 per cent ethyl alcohol. The purified 3,5-dinitrobenzoic acid weighs 57-61 g. (54-58 per cent of the theoretical amount) and melts at 205.-207° (Note 3). 

Ethyl-3,4-dinitrobenzoate, mp 71°. It may be prepd from the acid and alcohol with HQ gas-from the acid chloride and ethanol... 

In this paper, we first present a model study on blending a a,co-3,5-dinitrobenzoate PDMS and free 9H-carbazole-9-ethanol, in order to check whether the recently proposed 1 1 stoechiometry between carbazole and dinitrobenzoate molecules indeed applies (Scheme 1). [26] Then, we describe the preparation of triblock copolymers, poly[2-(N-carbazolyl)ethyl methacrylate]-fc-PDMS-fc-poly[2-(N-carbazolyl)ethyl methacrylate] (P(CzEMA)-fe-PDMS-fc-P(CzEMA)), using Atom Transfer Radical Polymerization (ATRP), and their blending with the acceptor-functionalized PDMS. In both studies, the physical association and thermal reversibility of these were followed by different techniques, including UV-Vis spectroscopy, DSC or Rheology. 

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