C Experimental Procedure

In particular we thought it would be useful to include cross-references of functional group transformations and an experimental procedure, so that the reader will be able to evaluate the reaction conditions at a glance for instance is this reaction carried out at room temperature or at 200 C For 1 h or 5 days Are special catalysts required How is the reaction worked up, what yield can be expected ... 

The synthetic procedure described is based on that reported earlier for the synthesis on a smaller scale of anthracene, benz[a]anthracene, chrysene, dibenz[a,c]anthracene, and phenanthrene in excellent yields from the corresponding quinones. Although reduction of quinones with HI and phosphorus was described in the older literature, relatively drastic conditions were employed and mixtures of polyhydrogenated derivatives were the principal products. The relatively milder experimental procedure employed herein appears generally applicable to the reduction of both ortho- and para-quinones directly to the fully aromatic polycyclic arenes. The method is apparently inapplicable to quinones having an olefinic bond, such as o-naphthoquinone, since an analogous reaction of the latter provides a product of undetermined structure (unpublished result). As shown previously, phenols and hydro-quinones, implicated as intermediates in the reduction of quinones by HI, can also be smoothly deoxygenated to fully aromatic polycyclic arenes under conditions similar to those described herein. 

Experimental procedures A The substance is dissolved or suspended in ether and treated with ethereal diazomethane. B The substance is dissolved in methanol (or ethanol, acetone, chloroform) and reacted with ethereal diazomethane. C A solution or suspension of the substance in ether is mixed with ethereal diazomethane,... 

The experimental procedure consisted of casting the varnish on glass plates by means of a spreader bar having an 0-102 mm (0 004 in) gap this produced a wet film 0-051 mm (0-002 in) thick that yielded a dried film of 0-025 mm (0-001 in). This standard thickness was used throughout and resistances are quoted in cm. The cast films were dried for 48 h in a glove box followed by a further 48 h in an oven at 65°C. 

General Experimental Procedures. Charge 1.0 eq. of substrate, 0.005 eq. or less catalyst, 8 volumes of dichloromethane, 8 volume of methanol. Purge the system three times each with nitrogen and hydrogen. Maintain the temperature at 25°C and hydrogen pressure at 45 psig, until the reaction is deemed complete. 

The bed void fraction and the Reynolds number were determined with the experimental procedures reported in literature [7]. Inprehminaty experiments, citral hydrogenation was investigated in six parallel reactors under identical reaction conditions, i.e., at 25°C and 6.1 bar hydrogen with the residence time of 156 s. The... 

Polymer preparation. PV0CC1 sample has been prepared by free-radical polymerization of pure V0CC1 (acquired from the SNPE, purity 99 ) in CH2CI2 at 35°C using dicyclohexyl peroxydicarbonate as initiator. The experimental procedure has been described previously ( 18, 1 9). The molecular weight Mn of this sample is equal to 50,000. 

Figures 5 and 6 show that there is a good correlation between the percentage conversion and the H/C atomic ratio of the coals for both experimental procedures.

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