The largest database of trusted experimental protocols

3 protocols using rh2 oac 4

1

Rhodium-Catalyzed C-H Amination Synthesis

Check if the same lab product or an alternative is used in the 5 most similar protocols
The solvents acetonitrile, N,N-dimethylformamide (DMF), dichloromethane, diethyl ether, and chlorobenzene were purchased from Fisher Scientific or Sigma Aldrich. Prior to use, the solvents were distilled over calcium hydride or filtered over dried alumina and stored over molecular sieves. Benzo[c]cinnoline (bncn) and p-toluenesulfonic acid (TsOH) were purchased from Sigma-Aldrich, Rh2(OAc)4 (OAc = acetate) and 1-benzyl-1,4-dihydronicotinamide (BNAH) were obtained from TCI. Cobaltocene was stored in a glove box preventing it from exposure to moisture and oxygen. Synthetic procedures were performed under a N2 atmosphere and the purification processes were opened to air; the general procedure is shown in Scheme S1 and 1H NMR spectra of the starting materials and products are shown in Fig. S1–S6 (ESI). The ligands diphenylbenzamidine (DPhB) and diphenyltriazenide (DPhTA), as well as the precursor cis-[Rh2(DPhTA)2(CH3CN)6][BF4]2 were synthesized according to literature procedures.37,38 (link)
+ Open protocol
+ Expand
2

Mass Spectrometric Analysis of Rh2(OAc)4 Binding to Metallothionein

Check if the same lab product or an alternative is used in the 5 most similar protocols
Solutions of Rh2(OAc)4 (Sigma-Aldrich) were
prepared in deoxygenated, argon-aerated, deionized water. Aliquots
containing known molar equivalents were added to the apo-MT solution
immediately prior to mass spectral data acquisition using a micrOTOF
II (Bruker Daltonics, Toronto). All solutions were at room temperature
and thoroughly deaerated using vacuum evacuation followed by Ar saturation.
NaI was used as the calibrant. Spectra were collected in positive
ion mode, as a function of time following mixing. The settings used
are described in the Supporting Information. The averaged spectra and data analysis were carried out using the
maximum entropy application in Bruker DataAnalysis 4.2 program. The
resulting spectral data were normalized, and the dominant species
were identified by mass.
+ Open protocol
+ Expand
3

Synthesis of Diazoacetates and Reagents

Check if the same lab product or an alternative is used in the 5 most similar protocols
Tetrahydrofuran
(THF) and toluene were dried
over a Na/K alloy and Na, respectively, and distilled before use.
CH2Cl2 was dried over CaH2 and used
without further purification. Cu(acac)2 (TCI; >97%),
Rh2(OAc)4 (AZmax; 99%), RuCl(cod)Cp* (Sigma-Aldrich),
Grubbs first catalyst (Sigma-Aldrich; 97%), 1-hexanol (TCI; >98.0%),
diisopropyl azodicarboxylate (Wako; >90%), triphenylphosphine (Nacalai;
>98.0%), MgCl2 (Nacalai; >97.0%), 1,8-diazabicyclo[5,4,0]-7-undecene
(DBU) (Nacalai; >97.0%), and 1-dodecanol (TCI; >99.0%) were
used as
received without further purification. Tosyl azide,27 4,4′-biphenylenediacetic acid,28 (link) 1,4-phenylenediacetic acid,28 (link),29 (link) and 2,2′-(9,9-dioctyl-9H-fluorene-2,7-diyl)diacetonitrile30 (link) were prepared following the procedures reported in the literatures.
Methyl 2-diazo-2-phenylacetate17 (link) was prepared
using tosyl azide as a diazo transfer agent following a reported general
procedure for this type of diazoketones. Caution! Extra care must
be taken for the preparation and handling of the diazoacetates because
of their potential explosiveness.
+ Open protocol
+ Expand

About PubCompare

Our mission is to provide scientists with the largest repository of trustworthy protocols and intelligent analytical tools, thereby offering them extensive information to design robust protocols aimed at minimizing the risk of failures.

We believe that the most crucial aspect is to grant scientists access to a wide range of reliable sources and new useful tools that surpass human capabilities.

However, we trust in allowing scientists to determine how to construct their own protocols based on this information, as they are the experts in their field.

Ready to get started?

Sign up for free.
Registration takes 20 seconds.
Available from any computer
No download required

Sign up now

Revolutionizing how scientists
search and build protocols!