The preparation of anhydrous inorganic chlorides by dehydration with thionyl chloride

Freeman, Jim; Smith, M.L.

doi:10.1016/0022-1902(58)80073-1

Cited by 132 publications

(36 citation statements)

References 5 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…All glassware was oven-dried at 140 C for at least 24 h, assembled while hot, and cooled under vacuum prior to use. The starting materials potassium phenylacetylide [10] and anhydrous CeCl 3 [13] were prepared according to the literature procedures. NMR spectra were recorded in THF-d 8 or C 6 D 6 solutions on a Bruker DPX 400 spectrometer at 25 C. Chemical shifts were referenced to TMS.…”

Section: General Proceduresmentioning

confidence: 99%

Synthesis and structural characterization of a homoleptic cerium(III) propiolamidinate

Dröse

Hrib

Edelmann

2010

Journal of Organometallic Chemistry

View full text Add to dashboard Cite

Section: General Proceduresmentioning

confidence: 99%

Synthesis and structural characterization of a homoleptic cerium(III) propiolamidinate

Dröse

Hrib

Edelmann

2010

Journal of Organometallic Chemistry

View full text Add to dashboard Cite

“…5,10,15,20-Tetra(4-carboxyphenyl)porphyrin (H 2 TPP(COOH) 4 , 1 ) was synthesized according to [33] and MCl 2 · n H 2 O salts (M = Zn II , Cu II , Ni II , Co II ) were dried according to [34]. …”

Section: Methodsmentioning

confidence: 99%

Synthesis, spectroscopic characterization and thermogravimetric analysis of two series of substituted (metallo)tetraphenylporphyrins

Al-Shewiki¹,

Mende²,

Buschbeck³

et al. 2017

Beilstein J. Nanotechnol.

View full text Add to dashboard Cite

Subsequent treatment of H2TPP(CO2H)4 (tetra(p-carboxylic acid phenyl)porphyrin, 1) with an excess of oxalyl chloride and HNR2 afforded H2TPP(C(O)NR2)4 (R = Me, 2; iPr, 3) with yields exceeding 80%. The porphyrins 2 and 3 could be converted to the corresponding metalloporphyrins MTPP(C(O)NR2)4 (R = Me/iPr for M = Zn (2a, 3a); Cu (2b, 3b); Ni (2c, 3c); Co (2d, 3d)) by the addition of 3 equiv of anhydrous MCl2 (M = Zn, Cu, Ni, Co) to dimethylformamide solutions of 2 and 3 at elevated temperatures. Metalloporphyrins 2a–d and 3a–d were obtained in yields exceeding 60% and have been, as well as 2 and 3, characterized by elemental analysis, electrospray ionization mass spectrometry (ESIMS) and IR and UV–vis spectroscopy. Porphyrins 2, 2a–d and 3, 3a–d are not suitable for organic molecular beam deposition (OMBD), which is attributed to their comparatively low thermal stability as determined by thermogravimetric analysis (TG) of selected representatives.

show abstract

“…The complexes Ln[NA C H T U N G T R E N N U N G (SiMe 3 ) 2 ] 3 (LnN'' 3 ) were made according to a literature procedure [32] from the chlorides. [33] All NMR spectra were recorded on a Bruker DPX 300 spectrometer, operating frequency 300. Preparation of (R)-[Y(L 1 ) 2 (OC 6 H 3 -tBu 2 -2,6)] (3a): A teflon tap-equipped NMR tube was charged with HOC 6 H 3 -tBu 2 -2,6 (8.1 mg, 0.04 mmol) and two equivalents of R-HL 1 (20.0 mg, 0.08 mmol), and C 6 D 6 (0.3 mL).…”

Section: Methodsmentioning

confidence: 99%

Ligand Recognition Processes in the Formation of Homochiral C₃‐Symmetric LnL₃ Complexes of a Chiral Alkoxide

Arnold

Buffet

Blaudeck

et al. 2009

Chemistry A European J

View full text Add to dashboard Cite

The reaction of a chiral racemic bidentate ligand HL1 (tBu2P(O)CH2CH(tBu)OH) with mid to late trivalent lanthanide cations affords predominantly homochiral lanthanide complexes (RRR)-[Ln(L1)3] and (SSS)-[Ln(L1)3]. A series of reactions are reported that demonstrate that the syntheses are under thermodynamic control, and driven by a ligand 'self-recognition' process, in which the large asymmetric bidentate L1 ligands pack most favourably in a C3 geometry around the lanthanide cation. The synthesis of bis(L1) adducts [Ln(L1)2X] (X=N(SiMe3)2, OC6H3tBu-2,6) is also reported. Analysis of the diastereomer mixtures shows that homochiral (L1)2 complexes are favoured but to a lesser extent. The complexes Ln(L1)3 and [Ln(L1)2(OC6H3tBu-2,6)] have been studied as initiators for the polymerization of epsilon-caprolactone and its copolymer with lactide, glycolide and its copolymer with lactide, and epsilon-caprolactam.

show abstract

The preparation of anhydrous inorganic chlorides by dehydration with thionyl chloride

Cited by 132 publications

References 5 publications

Synthesis and structural characterization of a homoleptic cerium(III) propiolamidinate

Synthesis and structural characterization of a homoleptic cerium(III) propiolamidinate

Synthesis, spectroscopic characterization and thermogravimetric analysis of two series of substituted (metallo)tetraphenylporphyrins

Ligand Recognition Processes in the Formation of Homochiral C₃‐Symmetric LnL₃ Complexes of a Chiral Alkoxide

Contact Info

Product

Resources

About

The preparation of anhydrous inorganic chlorides by dehydration with thionyl chloride

Cited by 132 publications

References 5 publications

Synthesis and structural characterization of a homoleptic cerium(III) propiolamidinate

Synthesis and structural characterization of a homoleptic cerium(III) propiolamidinate

Synthesis, spectroscopic characterization and thermogravimetric analysis of two series of substituted (metallo)tetraphenylporphyrins

Ligand Recognition Processes in the Formation of Homochiral C3‐Symmetric LnL3 Complexes of a Chiral Alkoxide

Contact Info

Product

Resources

About

Ligand Recognition Processes in the Formation of Homochiral C₃‐Symmetric LnL₃ Complexes of a Chiral Alkoxide