Yield, toluene

The synthesis of 9H-benzo[2,l-e]thiazolo-[2,3-c]-as-triazine (401) was achieved by oxydative cyclization of 2-imino-3-(o-aminophenyl)-4-phenyl-4-thiazoline (718, 719). This latter reacts also with paraformaldehyde in hot toluene yielding 3-phenyl-9H.10H-benzo[l,2-/]thiazolo-[2,3-d][l,3,5]triazepine (402) (720). This heterocyclic sytem is also formed when carboxylic acids replace paraformaldehyde (Scheme 230) (721). 

Hydrogenation Reactions. Hydrogen over a nickel, platinum, or paladium catalyst can partially or totally saturate the aromatic ring. Thermal hyrogenolysis of toluene yields benzene, methane, and biphenyl. 

The rhodium(II) acetate catalyzed reaction of 2-(3-oxo-2-diazobutyryl)-1,2,3,4-tetrahydroisoquinoline in boiling toluene yielded 2-methyl-4,6,7,l 16-tetra-hydro[l, 3]oxazino[2,3-n]-isoquinoline-4-one in 72% yield (99TL8269). 

A mixture of 5.2 parts of 4-chloro-3-nitrobenzophenone, 5 parts of ammonia, 72 parts of methanol and 13 parts of sulfolane is heated overnight at 125°C in a sealed tube. The reaction mixture is evaporated in vacuo. The semisolld residue is boiled in 100 parts of a diluted hydrochloric acid solution. After cooling, the precipitated product Is filtered off and dissolved in chloroform. The chloroform phase is dried and evaporated. The residue is crystallized from toluene, yielding 4-amino-3-nitrobenzophenone MP 141°C. 

Anhyd NH3(g) was bubbled through a stirring mixture of 6,7-di(phenylselanyl)naphthalene-2,3-dicarbo-nitrile (200 mg, 0.43 mmol), NaOMe (0.22 mmol) and 2-methoxyelhanol (5 mL) for 30 min. With continued NH3 introduction, the mixture was heated to 65 "C for 3 h. The solution was evaporated in vacuo. CuCl (21.8 mg, 0.22 mmol) and quinoline (5 mL) were added to the residue and refluxed for 2 h. MeOH was added and the precipitate was filtered, washed with acetone, CH2C12. and toluene yield 105 mg (51 %). 

Red Water — which can be almost black at times - also contains dissolved TNT however, it is not an incidental stream like Pink Water it is a major by-product stream from TNT manuf. The mixed-acid nitration of toluene yields not only 2,4,6-trinitrotoluene, the desired product, but also a host of other isomers and by-products amounting to approx 4.5% of the total yield and it is necessary to remove them from the product. They are removed by extraction with a Na sulfite—Na carbonate soln which sulfonates and dissolves them the extract is called Red Water. Red Water is a very complex and somewhat variable mixt containing 15% or so of sulfonated or sellited nitrobodies and a number of inorganic salts. Typical components are w, NajSOj—NaS04, NaN02— NaNOj, sulfonated or... 

Polymerization of t-butyl methacrylate initiated by lithium compounds in toluene yields 100% isotactic polymers 64,65), and significantly, of a nearly uniform molecular-weight, while the isotactic polymethyl methacrylate formed under these conditions has a bimodal distribution. Significantly, the propagation of the lithium pairs of the t-Bu ester carbanion, is faster in toluene than in THF. In hydrocarbon solvents the monomers seem to interact strongly with the Li+ cations in the transition state of the addition, while the conventional direct monomer interaction with carbanions, that requires partial dissociation of ion-pair in the transition state of propagation, governs the addition in ethereal solvents. 

Abbreviations Cy, cyclohexylidene DNP, 2,4-dinitrophenyl Py, pyridine TIPS, -(PrOjSiOSilPrOj- rac., racemate r.t., room temperature A, reaction in dichloromethane B, reaction in benzene D, reaction in diglyme T, reaction in toluene. Yields are described in the order of products, drawn from the left to the right. The sum of the last two compounds. Inserted as a reference reaction. 

Pulse radiolysis is used also for preparation of excited states of dienes and polyenes. This is done by irradiation of the diene/polyene in toluene solution. The radiolysis of toluene yield high concentration of molecules in the triplet excited state of the solute. Wilbrandt and coworkers61 pulse-radiolysed 1 mM solution of al I -lrans-1,3,5-heptatriene in toluene solution and observed the absorption spectra of the triplet state of the heptatriene with a maximum at 315 nm. The same group62 produced and measured the absorption spectra of several isomeric retinals in their lowest excited triplet state by pulse irradiation of their dilute solution in Ar-saturated benzene containing 10 2 M naphthalene. Nakabayashi and coworkers63 prepared the lowest triplet states of 1,3-cyclohexadiene,... 

Two derivatives of a cyclosilyl ether 148 have been synthesized by a German team <1994TL4335>. The enolizable cyclic hydroxamic acid 147 when treated with 2equiv of lithium diisopropylamide followed by reaction with di-fert-butyldichlorosilane in toluene yielded the stable [l,3,4,2]dioxazasilolo[5,4-c][l,4]oxazine derivative 148. 

Ultrasonic treatment of a mixture of elemental gallium and iodine in toluene yields a light green insoluble product described as gallium(I) iodide [36], However, it now seems to be dear, as a result of several experimental observations, that a mixture of subiodides of gallium is actually formed. Nevertheless, the green powder behaves like Gal in many reactions and has also been employed for the synthesis of tetrahedral tetragallium dusters [Eq. (2)] [37, 38]. 

Of the olefins, ethylene has been most extensively studied (19, 21, 23-26, 36) it reacts most readily in base-catalyzed alkylations. In general temperatures of 150-200 are used with relatively low ethylene pressures (0-70 atm.). Benzylic hydrogens are replaced by ethyl groups i.e., toluene yields n-propylbenzene. Additional substitution on the a-carbon may yield 3-phenylpentane and 3-ethyl-3-phenylpentane [Reaction (3)]. 

Themal treatment of the dimeric species 279 brings about a rearrangement to tetramer 281 (equation 56). The structure of 281 can be characterized by H, C H, P H and Li NMR spectroscopies. Recrystallization of 281 from toluene yields solvated crystals of formula 281-3PhMe, which show a core 12-membered macrocycle of C, P and Li atoms according to XRD crystallography ... 

The same concentration of 3 and 4 in toluene yielded similar results to those obtained for DMF solutions (Table 2). Therefore, this study illustrates two important concepts (1) whether in polar or nonpolar solvent Deloxan THP II and MP are capable of removing Pd and (2) regardless of oxidation state of Pd, even if Pd(0) and Pd(II) species are present in the same process solution, Deloxan THP II and MP are effective at removing Pd to levels well within the regulation limits for API manufacture. 

The residue in the flask, which has become pink in color, is extracted at 85-95° with three 1500-cc. portions of toluene, and the united extracts are distilled under reduced pressure on the steam bath until no more moisture passes over with the vapor. The solution (2-2.5 h) is then allowed to cool, whereupon 385-390 g. of catechol separates in colorless plates melting at 104-105°. The mother liquor is further concentrated under reduced pressure and the residue finally distilled, pure catechol passing over at 124-125 °/12 mm. The distillate, on recrystallization from a small quantity of toluene, yields 8-10 g. of pure material. 

The aqueous residue from the three extractions with toluene yields, when the bulk of the water has been distilled off on the steam bath under reduced pressure, a further quantity of catechol by extraction with hot toluene, but the crystals so obtained are contaminated with a red impurity. It is therefore preferable to distil the entire residue, again collecting the fraction boiling at 124—1250/12 mm. and recrystallizing it from fresh toluene. In this way 295-305 g. of pure product is obtained. The forerun contains a little aqueous hydrobromic acid, which may be employed in a subsequent batch. The total yield of pure catechol is 690-705 g. (77-80 per cent of the theoretical amount). 

Resinoids are prepared by extracting plant exudates (balsams, oleo gum resins, natural oleo resins, and resinous products) with solvents such as methanol, ethanol, or toluene. Yields range from 50 to 95%. The products are usually highly viscous and are sometimes diluted (e.g., with phthalates or benzyl benzoate) to improve their flow and processing properties. 

A number of cyclopentadienyl-ffee amidoAn -cyclooctatetraene complexes have been reported. Sattelberger s group found that [An(cot)Cl2(thf)2] with 2Na[N(SiMe3)2] in toluene yielded the crystalline [An(cot) N(SiMe3)2 2], which for An = Th was X-ray-characterised as a four-legged piano stool , with the Th- -Centroid distance of 2.04 A, each amido ligand having one short Th- - -C contact (3.15 or 3.04 A). The compounds [U(cot)-... 

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