W. Kliegel et al., STRUCTURAL STUDIES OF ORGANOBORON COMPOUNDS .62. SYNTHESIS AND STRUCTURE OF VARIOUS N-ALKYLATED 1,3-DIOXA-4-AZA-2-BORACYCLOHEXANES, Canadian journal of chemistry, 72(10), 1994, pp. 2118-2130
The synthesis of a number of variously substituted N-alkyl 2-hydroxyam
inoalkanols 3 and their reactions with phenylboronic acid are detailed
. The crystalline products proved to be 1:2 condensates 4 in a few cas
es and 1:1 condensates 5 in all the other cases studied. Crystals of -
pentamethylene-1,3-dioxa-4-aza-2-boracyclohexane, 5l, are triclinic, a
= 11.540(2), b = 10.402(3), c = 8.440(2) Angstrom, a = 108.86(2)degre
es, beta = 97.62(2)degrees, gamma = 89.36(2)degrees, Z = 2, space grou
p P $$($) over bar 1; and those of hylene-2-phenyl-1,3-dioxa-4-aza-2-b
oracyclohexane) benzene solvate, 15a.C6H6, are monoclinic, a = 22.690(
1), b = 16.867(1), c = 8.4783(9) Angstrom, beta = 104.912(8)degrees, Z
= 4, space group C2/c. The structures were solved by direct methods a
nd refined by full-matrix least-squares procedures to R = 0.037 and 0.
035 (R(w) = 0.035 and 0.044) for 3190 and 2084 reflections with I grea
ter than or equal to 3 sigma(F-2). respectively.