Solvent-free process for the preparation of the beta crystalline modification of 2,2',2''-nitrilo(triethyl-tris-(3,3',5,5'-tetra-tert-butyl-1,1'-biphenyl-2,2'-diyl)phosphite)

摘要

A process for the prepn. of beta, triclinic form of 2,2',2"-nitrilo(triethyl -(3,3',5,5'-tris-tetra-tert.-butyl-1,1'-biphenyl-2,2'-diyl) phosphite of formula (I). The process comprises heating in a closed vessel under atmospheric pressure at 90-160 [deg]C for 10-20 mins., wherein (I) melts at 200-207 [deg]C. The cpd. has an X-ray diffraction pattern exhibiting lines of very high intensity at 8.4, and 17; lines of high intensity at 9.9, 10.6, 11.4, 17.5, 19.1, 20.2; lines of medium intensity at 4.6, 4.9, 7.1, 12.7, 13.2, 13.6, 15.3, 15.8, 16.4, 16.7, 18.4, 19.7, 21.7, 23.4; and lines of weak intensity at 7.8, 8.8, 9.4, 12, 14.1, 14.6, 21, 22.3, 22.8, 23.9, 24.7, 25.3, 25.5, 26.4, 27, 27.7, 28.4 and a relative absolute configuration of the three stereo axes of the di:benzo[d, f][1,3,2]di:oxa-phosphepin rings of R*, R*, S*.