Quarterly Journal of the Chemical Society of London, Volume 1, Pages 1-1364 |
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Page 224
... filtered off , m.p. 150 ° , [ a ] 27-37-4 ° ( c 3.02 in ethyl acetate ) . The filtrate was left overnight and a second , less pure crop was obtained which was purified by shaking for 20 min . with acetic anhydride ( 60 ml . ) . Addition ...
... filtered off , m.p. 150 ° , [ a ] 27-37-4 ° ( c 3.02 in ethyl acetate ) . The filtrate was left overnight and a second , less pure crop was obtained which was purified by shaking for 20 min . with acetic anhydride ( 60 ml . ) . Addition ...
Page 225
... filtered and slowly added with stirring to a solution of dibenzylamine ( 12 ml . ) in ether ( 30 ml . ) cooled in ice . Scratching caused the substance to crystallize . It was filtered off after 2 hr . at 0 ° ( 14 g . , 65 % ) , m.p. ...
... filtered and slowly added with stirring to a solution of dibenzylamine ( 12 ml . ) in ether ( 30 ml . ) cooled in ice . Scratching caused the substance to crystallize . It was filtered off after 2 hr . at 0 ° ( 14 g . , 65 % ) , m.p. ...
Page 454
... filtered . The resulting precipitate ( 0.55 g . ) was purified by dissolution in N - sodium hydroxide and re- precipitation with 2N - acetic acid followed by crystallisation from butan - 1 - ol ( 300 pts ) . This gave yellow needles of ...
... filtered . The resulting precipitate ( 0.55 g . ) was purified by dissolution in N - sodium hydroxide and re- precipitation with 2N - acetic acid followed by crystallisation from butan - 1 - ol ( 300 pts ) . This gave yellow needles of ...
Contents
By K C BASS and G M TAYLOR | 1 |
ether 100 ml was added slowly to a stirred solution | 4 |
Oxidative dimerisations of natural rethrolones and related compounds with manganese dioxide | 9 |
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Common terms and phrases
1,2-Benzoquinone acetic acid acetone added adduct aldehyde Amer amine aqueous ethanol aromatic atom azine benzanilide benzene benzyl bromide Calc carbonyl CH₂ Chem chloride chloroform chromatography cm.¹ compound crystallised cyclisation decomp decomposition derivatives dilute dimer distillation dried eluted ester ethanol ethyl acetate EtOH evaporated extracted with ether filtered Found fraction gave give heated under reflux hydrazine hydride hydrochloride hydrogen chloride hydrolysis i.r. spectrum imine iodide isolated ketone light petroleum b.p. lithium aluminium hydride log ɛ Mannich base mass spectrum MeOH methyl methylene mixed m.p. mmHg mmoles mole n.m.r. spectrum needles nitrogen nucleophilic Nujol obtained oxidation phenyl potassium protons pyridine quinone reaction mixture requires residue room temperature salt Scheme showed silica gel sodium hydroxide solution solvent spectra starting material stirred Table Tetrahedron washed white solid yield