Bis(2-bromoalkyl)malononitriles by Addition of ... - ACS Publications

added, the mixture was heated to 165", and treated dropwise, over a 2-hr. ... Bis(2-bromoalkyl)malononitriles by Addition of Dibromomalononitrile to A...
0 downloads 0 Views 397KB Size
BIS(2-BROM0ALKYL)MALONONITRILES

OCTOBER,1963

added, the mixture was heated to 165", and treated dropwise, over

a 2-hr. period, with one mole of dimethyl disulfide at such a rate that the reaction temperature was maintained above 150'. The mixture was stirred a t reIlux for an additional 14 hr. and the organic layer was withdrawn, washed with a small amount of saturated sodium sulfate solution, and fractionated. There was obtained 83 g. (21%) of 4-methylmercapto-3-creso1, b.p. 108109' (1 mm.); benzenesulfonate, m.p. 79-80'; phenyl carbamate, m.p. 106-107". 4-Methylmercaptophenol (Phosphoric Acid Method) .-A mixture of 45 g. of phosphorus pentoxide, 155 g. of 85% phosphoric ac