The steroid 3, with three independently-addressable, rigidly-positioned functional groups, has be... more The steroid 3, with three independently-addressable, rigidly-positioned functional groups, has been synthesized in an efficient, multi-gram sequence from inexpensive cholic acid 1. Compound 3 should prove valuable as a starting point for combinatorial libraries with preorganised, co-directed arrays of substituents.Graphic
Dalton transactions (Cambridge, England : 2003), Jan 26, 2016
The molecular structures of a number of solvates of the [2 + 2] Schiff-base macrocycles {[2-(OH)-... more The molecular structures of a number of solvates of the [2 + 2] Schiff-base macrocycles {[2-(OH)-5-(R)-C6H2-1,3-(CH)2][O(2-C6H4N)2]}2 (R = Me L(1)H2, tBu L(2)H2, Cl L(3)H2), formed by reacting 2,6-dicarboxy-4-R-phenol with 2,2'-oxydianiline (2-aminophenylether), (2-NH2C6H4)2O, have been determined. Reaction of L(n)H2 with two equivalents of AlR'3 (R' = Me, Et) afforded dinuclear alkylaluminium complexes [(AlR'2)2L(1-3)] (R = R' = Me (1), R = tBu, R' = Me (2), R = Cl, R' = Me (3), R = Me, R' = Et (4), R = tBu, R' = Et (5), R = Cl, R' = Et (6)). For comparative studies, reactions of two equivalents of AlR'3 (R' = Me, Et) with the macrocycle derived from 2,2'-ethylenedianiline and 2,6-dicarboxy-R-phenols (R = Me L(4)H2, tBu L(5)H2) were conducted; the complexes [(AlMe)(AlMe2)L(5)]·2¼MeCN (7·2¼MeCN) and [(AlEt2)2L(4)] (8) were isolated. Use of limited AlEt3 with L(3)H2 or L(5)H2 afforded mononuclear bis(macrocyclic) complexes [Al(L(3))...
... Preparation of New N-Heterocyclic Carbene Metal-Alkyne Complexes and Application to a Stereoc... more ... Preparation of New N-Heterocyclic Carbene Metal-Alkyne Complexes and Application to a Stereocontrolled Pauson-Khand Reaction. Andrew M. Poulton a , Steven DR Christie* a , RossFryatt a , Sophie H. Dale a , Mark RJ Elsegood a , David M. Andrews b,. ...
Phosphorus Sulfur and Silicon and the Related Elements, 2013
ABSTRACT A simple two-step route to a series of carboxylic acid functionalized ditertiary phosphi... more ABSTRACT A simple two-step route to a series of carboxylic acid functionalized ditertiary phosphine oxides is described, including the X-ray crystal structures of three representative examples namely {Ph2P(O)CH2}2N(CH2)nCO2H (n = 3−5). Strong intermolecular O−H···O H-bonding is observed in all cases leading to distinct packing arrangements.
Treatment of the ligands 3,5-tBu2-2-(OH)C6H2CHNR [R=2-(CO2H)C6H4 (1a) and 2-(CO2H)C10H6 (1b)] wit... more Treatment of the ligands 3,5-tBu2-2-(OH)C6H2CHNR [R=2-(CO2H)C6H4 (1a) and 2-(CO2H)C10H6 (1b)] with trimethylborate, B(OMe)3, in toluene yields, after work-up, the yellow crystalline complexes {[3,5-tBu2-2-(O)C6H2CHNR]B(OMe)} [R=2-(CO2)C6H4 (2a) and 2-(CO2)C10H6 (2b)], respectively. Further treatment of these complexes with trifluoromethanesulfonic (triflic) acid, CF3SO3H, followed by recrystallisation from tetrahydrofuran (thf) afforded the triflate salts [{3,5-tBu2-2-(O)C6H2CHNR}B(thf)][CF3SO3] [R=2-(CO2)C6H4 (3a) and 2-(CO2)C10H6 (3b)]. An electroluminescent device was constructed using 2a, which produced orange-green light with broad emission spectra (maximum brightness of 5cd/m2 being observed at 13V). Compounds 1a and 2b·2MeCN have been characterised by single crystal X-ray structure determinations.
The steroid 3, with three independently-addressable, rigidly-positioned functional groups, has be... more The steroid 3, with three independently-addressable, rigidly-positioned functional groups, has been synthesized in an efficient, multi-gram sequence from inexpensive cholic acid 1. Compound 3 should prove valuable as a starting point for combinatorial libraries with preorganised, co-directed arrays of substituents.Graphic
Dalton transactions (Cambridge, England : 2003), Jan 26, 2016
The molecular structures of a number of solvates of the [2 + 2] Schiff-base macrocycles {[2-(OH)-... more The molecular structures of a number of solvates of the [2 + 2] Schiff-base macrocycles {[2-(OH)-5-(R)-C6H2-1,3-(CH)2][O(2-C6H4N)2]}2 (R = Me L(1)H2, tBu L(2)H2, Cl L(3)H2), formed by reacting 2,6-dicarboxy-4-R-phenol with 2,2'-oxydianiline (2-aminophenylether), (2-NH2C6H4)2O, have been determined. Reaction of L(n)H2 with two equivalents of AlR'3 (R' = Me, Et) afforded dinuclear alkylaluminium complexes [(AlR'2)2L(1-3)] (R = R' = Me (1), R = tBu, R' = Me (2), R = Cl, R' = Me (3), R = Me, R' = Et (4), R = tBu, R' = Et (5), R = Cl, R' = Et (6)). For comparative studies, reactions of two equivalents of AlR'3 (R' = Me, Et) with the macrocycle derived from 2,2'-ethylenedianiline and 2,6-dicarboxy-R-phenols (R = Me L(4)H2, tBu L(5)H2) were conducted; the complexes [(AlMe)(AlMe2)L(5)]·2¼MeCN (7·2¼MeCN) and [(AlEt2)2L(4)] (8) were isolated. Use of limited AlEt3 with L(3)H2 or L(5)H2 afforded mononuclear bis(macrocyclic) complexes [Al(L(3))...
... Preparation of New N-Heterocyclic Carbene Metal-Alkyne Complexes and Application to a Stereoc... more ... Preparation of New N-Heterocyclic Carbene Metal-Alkyne Complexes and Application to a Stereocontrolled Pauson-Khand Reaction. Andrew M. Poulton a , Steven DR Christie* a , RossFryatt a , Sophie H. Dale a , Mark RJ Elsegood a , David M. Andrews b,. ...
Phosphorus Sulfur and Silicon and the Related Elements, 2013
ABSTRACT A simple two-step route to a series of carboxylic acid functionalized ditertiary phosphi... more ABSTRACT A simple two-step route to a series of carboxylic acid functionalized ditertiary phosphine oxides is described, including the X-ray crystal structures of three representative examples namely {Ph2P(O)CH2}2N(CH2)nCO2H (n = 3−5). Strong intermolecular O−H···O H-bonding is observed in all cases leading to distinct packing arrangements.
Treatment of the ligands 3,5-tBu2-2-(OH)C6H2CHNR [R=2-(CO2H)C6H4 (1a) and 2-(CO2H)C10H6 (1b)] wit... more Treatment of the ligands 3,5-tBu2-2-(OH)C6H2CHNR [R=2-(CO2H)C6H4 (1a) and 2-(CO2H)C10H6 (1b)] with trimethylborate, B(OMe)3, in toluene yields, after work-up, the yellow crystalline complexes {[3,5-tBu2-2-(O)C6H2CHNR]B(OMe)} [R=2-(CO2)C6H4 (2a) and 2-(CO2)C10H6 (2b)], respectively. Further treatment of these complexes with trifluoromethanesulfonic (triflic) acid, CF3SO3H, followed by recrystallisation from tetrahydrofuran (thf) afforded the triflate salts [{3,5-tBu2-2-(O)C6H2CHNR}B(thf)][CF3SO3] [R=2-(CO2)C6H4 (3a) and 2-(CO2)C10H6 (3b)]. An electroluminescent device was constructed using 2a, which produced orange-green light with broad emission spectra (maximum brightness of 5cd/m2 being observed at 13V). Compounds 1a and 2b·2MeCN have been characterised by single crystal X-ray structure determinations.
Uploads