Cupric Chloride → HCID 86662767, compound

Treatment of anhydrous copper(II) chloride with two equivalents of LtBu,NMe2K, LiPr,NMe2K or LMe,NMe2K, prepared in situ from the corresponding carbohydrazide ligands and potassium hydride, in tetrahydrofuran afforded the mononuclear copper(II) bis-carbohydrazide complexes Cu(LtBu,NMe2)2 (32, 75%), Cu(LiPr,NMe2)2 (33, 51%), and Cu(LMe,NMe2)2 (34, 23%), respectively, as maroon crystals (eq 9). Compound 32 was isolated in high yield from sublimation at 70° C./0.05 Torr, whereas sublimation yields for 33 (75° C./0.05 Torr) and 34 (80° C./0.05 Torr) were substantially lower. Similar treatment of cobalt(II) chloride with LtBu,NMe2K afforded Co(LtBu,NMe2)2 (35, 57%) as red crystals upon sublimation at 75° C./0.05 (eq 9). Treatment of the mono acetonitrile adduct of nickel(II) chloride with two equivalents of LtBu,NMe2K or LiPr,NMe2K afforded the mononuclear bis-carbohydrazide complexes Ni(LtBu,NMe2)2 (36, 76%) and Ni(LiPr,NMe2)2 (37, 62%), respectively, as orange color crystals upon sublimation at 70° C. and 80° C./0.05 Torr, respectively (eq 10).

ORD record

ord-2399acb94720470195f37bb7e789e0d2

Source dataset

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08962876B2