Melt extraction melting reactions

Thereafter, add and dissolve 14 grams of 2-amino-3,4,5,6-tetranitrotoluene (prepared in step 2) while stirring the acid mixture. Then slowly add 7 milliliters of 98% sulfuric acid, drop wise, over a period of 40 minutes while stirring the reaction mixture. After the addition of the 98% sulfuric acid, stir the reaction mixture overnight at room temperature. Afterwards, extract the reaction mixture with six 150-milliliter portions of chloroform. The chloroform will be the upper layer. After the extraction process, combine all three portions of chloroform (if not already done so), and then remove the chloroform by distillation at 65 Celsius until dry solid remains (the distillation may need to be temporarily stopped in order to filter-off precipitated product). After the chloroform has been removed, remove the heat source and allow the contents in the distillation flask to cool to room temperature. Then collect the dry product from the distillation flask, and then vacuum dry or air-dry any product that may have been filtered-off during the distillation process. Then combine all the dry product, wash with 400 milliliters of water, and then vacuum dry or air-dry. The result will be 13 grams of pentanitrotoluene, as yellow crystals with a melting point of 224 Celsius. 

Reduction to Amines. Place 100 mg of the unknown in a reaction tube, add 0.2 g of tin, and then—in portions—2 mL of 10% hydrochloric acid. Reflux for 30 min, add 1 mL of water, then add slowly, with good cooling, sufficient 40% sodium hydroxide solution to dissolve the tin hydroxide. Extract the reaction mixture with three 1-mL portions of ether, dry the ether extract over anhydrous sodium sulfate, wash the drying agent with ether, and evaporate the ether to leave the amine. Determine the boiling point or melting point of the amine and then convert it into a benzamide or acetamide as described under 4. Primary and Secondary Amines p. 587. 

Epoxy triazine-capped PC (50)/ acid- or anhydride-functionalized PO (50) Solution reaction/copolymer analysis by selective solvent extraction/numerous functionalized PO used/also used SMA in melt reaction in place of functionalized PO Brown et al. 1991a... 

The sodium fusion and extraction, if performed strictly in accordance with the above directions, should be safe operations. In crowded laboratories, however, additional safety may be obtained by employing the follow ing modification. Suspend the hard-glass test-tube by the rim through a hole in a piece of stout copper sheet (Fig. 69). Place 1 -2 pellets of sodium in the tube, and heat gently until the sodium melts. Then drop the organic compound, in small quantities at a time, down — =. the tube, allowing the reaction to subside after each addition before the next is made. (If the compound is liquid, allow two or three small drops to fall at intervals from a fine dropping-tube directly on to the molten sodium.) Then heat the complete mixture as before until no further reaction occurs. 

Y-Phenylbutyric acid. Prepare amalgamated zinc from 120 g. of zinc wool contained in a 1-litre rovmd-bottomed flask (Section 111,50, IS), decant the liquid as completely as possible, and add in the following order 75 ml. of water, 180 ml. of concentrated hydrochloric acid, 100 ml. of pure toluene (1) and 50 g. of p benzoylpropionic acid. Fit the flask with a reflux condenser connected to a gas absorption device (Fig. II, 8, l,c), and boil the reaction mixture vigorously for 30 hours add three or four 50 ml. portions of concentrated hydrochloric acid at approximately six hour intervals during the refluxing period in order to maintain the concentration of the acid. Allow to cool to room temperature and separate the two layers. Dilute the aqueous portion with about 200 ml. of water and extract with three 75 ml. portions of ether. Combine the toluene layer with the ether extracts, wash with water, and dry over anhydrous magnesium or calcium sulphate. Remove the solvents by distillation under diminished pressure on a water bath (compare Fig. II, 37, 1), transfer the residue to a Claisen flask, and distil imder reduced pressure (Fig. II, 19, 1). Collect the y-phenylbutyric acid at 178-181°/19 mm. this solidifies on coohng to a colourless sohd (40 g.) and melts at 47-48°. 

Method 2. Ethyl p-nitrobenzoate. Place 21 g. of p-nitrobenzoic acid (Section IV,154), 11-5 g. of absolute ethyl alcohol, 3 8 g. of concentrated sulphuric acid, and 30 ml. of sodium-dried A.R. benzene in a 250 ml. round-bottomed flask, fit a reflux condenser, and heat the mixture under reflux for 16 hours. Add 50 ml. of ether to the cold reaction mixture, wash the extract successively with sodium bicarbonate soiution and water, dry with anhydrous magnesium sulphate or calcium chloride, and distil off the solvent on a water bath. Remove the last traces of benzene either by heating in an open evaporating dish on a water bath or in a bath at 100-110°. The residual ethyl p-nitrobenzoate (21 g.) solidifies completely on cooling and melts at 56°. 

Thirty minutes after refluxing had stopped, a trace of copper(I) bromide was added to terminate the conversion. The reaction mixture was cautiously poured on to 500 g of finely crushed ice, then 200 ml of 4 N hydrochloric acid were added. After the remaining ice had melted the layers were separated and the aqueous layer was extracted three times with diethyl ether. The combined ethereal solutions were washed with saturated NaCl solution and dried over magnesium sulfate. The greater part of... 

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