Dinitro benzoates

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.)... 

Add 1 ml. of the alcohol-free ether to 0-1-0-15 g. of finely-powdered anhydrous zinc chloride and 0 5 g. of pure 3 5-dinitrobenzoyl chloride (Section 111,27,1) contained in a test-tube attach a small water condenser and reflux gently for 1 hour. Treat the reaction product with 10 ml. of 1-5N sodium carbonate solution, heat and stir the mixture for 1 minute upon a boiling water bath, allow to cool, and filter at the pump. Wash the precipitate with 5 ml. of 1 5N sodium carbonate solution and twice with 6 ml. of ether. Dry on a porous tile or upon a pad of filter paper. Transfer the crude ester to a test-tube and boil it with 10 ml. of chloroform or carbon tetrachloride filter the hot solution, if necessary. If the ester does not separate on cooling, evaporate to dryness on a water bath, and recrystallise the residue from 2-3 ml. of either of the above solvents. Determine the melting point of the resulting 3 5 dinitro benzoate (Section 111,27). 

Alcohol B.P. M.P, 3 5-Dinitro-benzoate p-Nilro- bemoate Phenyl- urethane a-Naph- thyl- urethane Hydrogen 3-nitro- phthalate other Derivatives... 

Alcohol B.P. Benzoate />-Nitro- benzoate S S-Dinitro- benzoate Phenyl- urethane a-Naphthyl. urethane Other Derivatives... 

Fig. 6 Differential scanning calorimetry thermogram of 2,4-dinitrophenyl-2,4-dinitro-benzoate, illustrating the recrystallization of form IV into form III (Tl), the melting of forms III and II (T2 and T4), the solidification of the melts produced by T2 and T4 (T3 and T5), and the melting of form I (T6). (Data adapted from Ref. 46.)...

Ethyl 4-amino-2-nitrobenzoate It yel ndls, mp 130° sol in ale, eth insol in w may be prepd from hydrazinehydrate and ethyl 2,4-dinitro-benzoate in abs ale or from 4-ami no-2 nitro-beazoic acid and ethyl iodide in ale potasb or ale sulfuric acid... 

Alcohol B.P. °C Benzoate °C p-NItro- benzoate °C 3,5-Dinitro- benzoate °C Phenyl- urethan °C 1-Napbthyl- urethan °C Other derivatives °C... 

Disulfides, 3,5-dinitro-benzoates Whatman 3 (impregnated with 10% paraffin oil in (CH2)e) DMF/MeOH/w or Foram/MeOH/w 58... 

Barborak and Schleyer (1970) also solvolyzed 4-deuterio-bicyclo[3.2.2]-nona-2,6,8-trien-4-yl-3,5-dinitrobenzoate [426] in 60% aqueous acetone. Two products were obtained in 1 1 ratio deuterated 9-barbaralyl dinitro-benzoate [427] formed by return and deuterated [425 X = OH]. No bicyclo-[3.2.2]nonatrien-2-ol product could be detected. The deuterium in [427] and... 

Amino Acid M.P. Benzoate 3 5-Dinitro-benzoate Phenyl-nreido Acid />-Toluene- sulphonate 2 4-Dichloro-phenoxy-acetate a-Naphthyl-nreido Acid Phthalyl Derivative... 

Name point c point c "S DP ihyl urethane Dinitro benzoate 3 nilro phihalale gen phthalate Miscellaneous... 

In the workup sequence, following concentration of the reaction solution and the addition of methanol, the sparingly-soluble 2 -diene components (lu-misterolj, lumisterol2,7-dehydrocholesterol, and ergosterol, respectively) can be removed by filteration. Tachysterolj is separated off in the form of its Diels-Alder adduct with maleic anhydride. The mother liquor is evaporated and maybe used directly as an additive for animal feed (Vitamin D3-resin). Vitamin D for the food and pharmaceutical sector is first purified as its butanoate or 3,5-dinitro-benzoate by recrystaUisation, and then hydrolysed and again recrystaUised. 

No Name Boiling point c Melting point c n20 DJ Phenyl urethane 1 Naph thyl urethane 4 Nitro benzoate 35 Dinitro benzoate Hydrogen 3 nuro phthalatc Hydro gen phthalatc Miscellaneous... 

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