Phloroglucinol methylene

Nitric acid, Sulfuric acid, Phloroglucinol, Hydrochloric acid Sodium chlorate. Copper sulfate. Ammonium hydroxide. Alcohol Sodium chlorate. Copper sulfate. Ammonium hydroxide. Alcohol Sulfuric acid. Potassium nitrate, 1,3,5-Trifluorobenzene, Methylene chloride. Hexane, Charcoal, Sodium sulfate, 2-Amino-2-methylpropanone, Potassium hydrogen carbonate, 1,2-Dichloroethane, Trifluoroacetic acid. Urea, Dimethylformamide Nitric acid. Urine... 

The spectra of 0-Time samples generally contained only about 80% of the expected methylol protons, probably due to more hydration of the benzyl alcohols than the resorcinol or phloroglucinol. Also, some samples showed the presence of small amounts of methylene linkages due to some self-condensation of the hydroxybenzyl alcohols prior to their reaction with either resorcinol or phloroglucinol. Therefore, calculations of the number of methylols lost and... 

In reactions at pH 11.0, no phloroglucinol A-ring can be detected after only 1 hour at 100 °C, and there is little change in the amount of methylol or formation of methylene bridge after 6 hours of heating. The methylene signals that are... 

Table V. Methylol, Methylene, and Degree of Substitution per Mole of Phloroglucinol after Reaction with o- and p-IIydroxybenzyl Alcohols...

The existence of the dianion 19 was proved by means of NMR spectroscopy . Thus, the H NMR spectrum of phloroglucinol in aqneons solntion contains a single resonance of aromatic protons (S 6.05) which shows a small shift to high field (S 6.02) after addition of one mole of an alkali. However, the addition of a second mole of alkali results in the disappearance of the aromatic proton signal. Instead of Ihis, olefinic proton signals (5 5.03) as well as signals of the methylene protons (5 3.0) appear. 

At the time of its discovery there was not available enough d-isocory-palmine for the determination of its structure by degradative methods, but Spath and Mosettig (231) prepared it from d-canadine by, first, de-methylenation to XiXXVI (2,3-dihydroxy-9,10-dimethoxytetrahydro-protoberberine, m.p. 252-253°) by means of phloroglucinol and sulfuric acid and, then, by incomplete methylation with diazomethane. In addition to the non-phenolic tetrahydropalmatine, there was formed a separable mixture of d-corypalmine and d-isocorypalmine (XXXVTI),... 

It is interesting to note that while -CH2-O-CH2- ether bridged compounds have been isolated for the phenol-formaldehyde [24] reaction, their existence for fast-reacting phenols such as resorcinol and phloroglucinol has been postulated, but they have not been isolated, as these two phenols have always been considered too reactive with formaldehyde. They are detected by a surge in the concentration of formaldehyde observed in kinetic curves due to methylene ether bridge decomposition [19]. 

Because methylene blue is a cationic dye, it would be expected to have activity as a Lewis acid. The correlation with methylene blue was weak but showed the expected trend, with increased methylene blue binding being negatively correlated to increased Phloroglucinol and isovanillic acid were the only laccase substrates that increased the ATp of the fiber. All substrates other than resorcinol, 4-hydroxyphenylacetic acid, 1,2,3-trihydroxybenzene, and 1,2,4-... 

Several ferns, mostly those of the genus Dryopteris, elaborate compounds in which methylated phloroglucinol units (such as 38) are coupled through methylene groups to yield... 

Preparation by reaction of 2,4-dichloroben-zoyl chloride with 0,0,0-tris(trimethylsilyl) phloroglucinol in the presence of stannic chloride in refluxing methylene chloride for 2 h (76%) [921]. 

Preparation by hydrogenolysis of 2,2, 4, 6-tetrakis-(benzyloxy)-4 -methoxy-6 -methylbenzophenone (SM) in ethyl acetate/tetrahydrofuran mixture in the presence of 10% Pd/C at 25°. SM was obtained by condensation of 2-(benzyloxy)-4-methoxy-6-methyl-benzoic acid with phloroglucinol tribenzyl ether in the presence of trifluoroacetic anhydride in methylene chloride under nitrogen for 15 min (81%) [1179]. 

Preparation by reaction of acetic acid on phloroglucinol with zinc chloride (Nencki reaction), and then saponification of 5,7-dihydroxy-4-methylene-2-(2,4,6-trihydroxyphenyl)-4//-benzopyran first formed (76%) [2429],... 

The reactivity of the amino group can be strongly influenced by the presence of negative substituents in the amine molecule. For example, trinitroaniline and trichloroaniline do not react. On the other hand, in addition to primary aliphatic amines, aromatic amines, and amino acids, substances with an active methylene group also react (3). A positive reaction was also observed with substances such as guanidine, semicarbazide, phenyl-hydrazine, ethyleneimine, piperidine, piperazine, benzylcyanide, cyano-acetylacetone, diethyl malonate, ethyl acetoacetate, dibenzoylmethane, rhodanin, indole, methylphenylpyrazolone, resorcinol, phloroglucinol, and quaternary heterocyclic bases and oxonium salts. 

---