4-Biphenylcarbonyl chloride

Cl Vat YeUow 12 is prepared by condensing l-anaino-5-ben2oylaininoanthraquinone [117-06-6] (161) with oxalyl chloride in nitroben2ene. Cl Vat YeUow 33 is prepared by condensation of two moles of 1-aminoanthraquinone with one mole of 4V -a2obis(4-biphenylcarbonyl chloride). Cl Vat Red 21 is prepared from 1,4-diaminoanthraquinone (33) and l-nitroanthraquinone-2-carboxyhc acid (58) by the foUowing process ... 

Biphenylcarbonyl chloride [14002-51-8] M 216.7, m 114-115 . Dissolve in a large volume of pet ether (10 x, b 50-70 ), filter through a short column of neutral alumina, evaporate to dryness in vacuo and recryst from pet ether (b 60-80 ). LACHRYMATORY. 

The 1,3,2,4,6-dithiatriazine 21 (Ar=Ph) is inert to concenttated hydrochloric acid and TFA in dichloromethane at room temperature and does not react with 4-biphenylcarbonyl chloride in the presence of triethylamine <19%JHC295>. 

The procedure for derivative preparation was that described by Jungalwala et al. (1975). Standards (10-100 nmol) were dried and 50 pi of 1% solution of 4-biphenylcarbonyl chloride in tetrahydrofurane was added, (4-biphenylcarbonyl chloride was obtained from Aldrich Chemical Co., Milwaukee, Wi. U.S.A.) followed by 100 pi of aqueous 50% sodium acetate solution. The mixture was shaken vigorously at room temperature for sixty minutes. The reaction products were purified as follows 5 ml of lower phase (1 vol. of chloroform methanol 2 1 was equilibrated with 0.2 vol. of water, the phases separated and the upper phase was discarded) was added to the reaction mixture and the excess of reagent was removed by washing three times with 1 ml of methanol water chloroform 15 M-NH3 (96 92 2 3). The lower phase was evaporated to dryness under N2 and the residue was then dissolved in 250 pi of chloroform methanol 1 1. 

Preparation by reaction of 4-biphenylcarbonyl chloride with resorcinol dimethyl ether in the presence of aluminium chloride [408],... 

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