Ethyl Tosyl-L-isoleucylg1ycinate.-A solution of tosyl-Lisoleucyl chloride (prepared from 2.9 g. of tosyl-L-isoleucine and-phosphorus pentachloride) in r5 ml. of anhydrous ether was added slowly to a suspension of 2.5 g. of ethyl glycinate hydrochloride and 3.5 ml. of triethylamine in 50 ml. of anhydrous ether and the mixture was allowed to stand at room temperature for 12 hours. The white precipitate was filtered off and washed with ether. After trituration with water to remove the triethylamine hydrochloride, 3.34 g. of product, m.p. 159-160°, was obtained; yield 89%. Another 0.25 g., m.p. 152-154', was afforded by extraction of the ether filtrate successively with water, dilute HCl, dilute aqueous KHCO, and water, followed by removal of the ether zn vacuo. Recrystallization of the second crop from ethanol raised the m.p. to 158-160". For analysis, the tosyl dipeptide ester was recrystallized twice from ethanol and then melted a t 160-161".
Orthophosphoric acid has been found to accomplish the previously unsuccessful oyclization of azomethines of 3-formylcarbazoles and aminoacetal to substituted pyrido[4,3-b]carbazoles according to a scheme proposed by Cranwell and Sexton. By this method, there have been prepared 6,ll-dimethyl-(ellipticine), 5,6,11trimethyl-, 5,9,11-trimethyl-, 9-methoxy-5,ll-dimethyl-(9-methoxyellipticine), 9-methoxy-5,6,11-trimethyl-, 9-bromo-6,ll-dimethyl-, and 9-nitro-5,ll-dimethyl-6H-pyrido[4,3-blcarbazole.
Alcohols and phenols are phosphorylated in
high yield by reaction with various 2-chloroalkylphosphonic acids at 20-50�C in
the presence of three or more molar equivalents of cyclohexylamine or
triethylamine, the other products being the corresponding alk-1-ene and
chloride ion. The reaction probably proceeds by attack of an ROH molecule on
the phosphorus atom of a doubly-ionized phosphonate group.
2-Chlorodecyl-, 10-carboxy-2-chlorodecyl-,
and 2-chloro-octylphosphonic acid decompose rapidly in neutral solution giving
chloride ion, phosphate ion, and the corresponding alk-1-ene. In the absence of
hydroxylic compounds, 2-chlorodecylphosphonic acid is decomposed by
cyclohexylamine to dec-1-ene and a product which appears to be
N-cyclohexylphosphoramidate; t-amines and also aniline cause
dehydrohalogenation to dec-1-enylphosphonic acid.
The proton magnetic resonance spectra of
most of the phosphorus-containing substances described herein are recorded.
Gold(1) complexes of type RsAuX (R = Bu, Ph; X = C1, Br, SCN), complexes PhsPAuSR (R = alkyl, aryl), PhsPAuEt, (PhO)sPAuCl, and bis(phosphine) complexes of type [R3PAuPRs]fX-(R = Et, Ph; X = C1, Br, SCN) are described. Triphenyl phosphite complexes were very unstable; attempts to prepare triethyl phosphite complexes were unsuccessful. A triethylphosphine complex of aurous sulphide, EtsPAuSAuPEts, and a sulphonium complex, [(Ph3PAu)3S]+C1-, were also prepared.
kindly provided by Allied Chemical Corp., N.Y., U.S.A.) (1.66 g.) and toluene-p-thiol (1.29 g . ) were heated together Minoura, J. SOC. Rwbber I n d .Acetyl o-Nitrophenyl DisuZphide.-Thiolacetic acid (4 g.) in water (20 ml.) was titrated to pH 7 with 10N-sodium hydroxide, and the solution made into a slurry with o-nitrobenzenesulphenyl chloride (5.5 g.). After 5 min. the mixtiire was filtered and the precipitate
Support for this mechanism has now been obtained by allowing dimethyl trisulphide to react with sulphite ion at pH 8; considerable amounts of dimethyl disulphide were formed.
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