Propylamine method

Treatment of oc-cyclopropyl ketones with lithium in a mixture of N,N-d2 propylamine and hexamethylphosphortriamide is a recently reported method for deuterium labeling via reductive ring opening. This reaction provides y-labeled ketones in good yield (70-100%) and isotopic purity (85-93%). 

Amino acids labeled with DNS-C1 were determined using the Ru(bpy)32+ CL reaction after HPLC separation with a reversed-phase column [104, 105], DNS derivatives are expected to produce intense CL owing to their secondary and tertiary amino groups. The detection limit for DNS-Glu was 0.1 pM (2 pmol/ injection). Although underivatized amino acids could be detected by Ru(bpy)32+ CL, the DNS derivatives showed improved detection limits by three orders of magnitude [105], An approach to convert primary amines to tertiary amines was also reported [106], In this method, divinyl sulfone (DVS) was used for a cycloaddition reaction of primary amines (Fig. 19). The DVS derivatives after HPLC separation were sensitively detected (e.g., detection limits for propylamine and 3-aminopentane were 30 and 1 pmol, respectively). 

An EPA method was created for measuring NDMA and six additional nitrosamines in drinking water (EPA Method 521) [55]. This method uses GC/ chemical ionization (CI)-MS/MS and enables the measurement of NDMA and six other nitrosamines (N-nitrosomethylethylamine, N-nitrosodiethylamine, N-nitroso-di-n-propylamine, N-nitroso-di- -butylamine, N-nitrosopyrrolidine, and N-nitrosopiperidine) in drinking water at detection limits ranging fi om 1.2 to 2.1 ng/L. A liquid chromatography (LC)/MS/MS method [56] can also be used to measure nine nitrosamines, including N-nitrosodiphenylamine, which is thermally unstable and cannot be measured using the EPA Method. 

Desipramine Desipramine, 10,1 l-dihydro-5-[3-(methylamino)propyl]-5H-dibenz[b,f] azepine (7.1.13), differs from imipramine in that it contains only one methyl group on the nitrogen atom of the propylamine side chain. The suggested methods of desipramine synthesis are very simple, and the difference lies only in the manner in which the secondary methylamine group is introduced into the structure of the drug. 

The second method nses the same reagents in the presence of a base and consists of initially making 3-(l-naphthyloxy)propylenoxide (12.1.3), the snbseqnent reaction with iso-propylamine which resnlts in epoxide ring opening leading to the formation of propranolol (12.1.2) [1-6]. 

AIPO4-5 molecular sieve (BET surface area, 299 m g ) used in this study was prepared by the method of Wilson et al. [1j. VjOg/AIPO -S samples were prepared by impregnating with aqueous solutions of ammonium vanadate after removing templating agent in the AIPO -S by calcining at 530°C. The samples were dried at 110 C for 24 h then calcined in air at 550°C for 2 h. VAPO -S was prepared from gel mixture of phosphoric acid, pseudoboehmite, vanadium pentoxide, tri-propylamine and water (1.3 PrjN x AljOj PjOj 40 HjO) by crystallization at 165°C for 3 - 7 days [7. ... 

Like the oxa method for naming ethers (Problem 14.61), the aza method is used for amines. Di-n-propylamine, CH3CH2CH2NHCH2CH2CH3, is 4-azaheptane and piperidine is azacyclohexane. The four H s of NH can be replaced to give a quaternary (4°) tetraalkyl (tetraaryl) ammonium... 

A wide variety of amines, including aryl alkyl amines, alkyl amines, and amino alcohols have been resolved on a multi-ton scale (Scheme 7.10) [7]. This method has been used with methyl ethers. For example the racemic (l-methoxy)-2-propylamine (R,S 19) can be separated to give the (S)-20 which is required for the synthesis of a corn herbicide (21) and produced at 2500 t/y [7, 30] (Scheme 7.11). 

The sensor did not respond to volatile compounds such as acetic acid, ethyl alcohol, and amines (diethylamine, propylamine, and butylamine) or to nonvolatile nutrients such as glucose, amino acids, and metal ions (potassium and sodium ions). Therefore, the selectivity of this microbial sensor was satisfactory in the presence of these different substances. The current output of the sensor was almost constant for more than 21 days and 400 assays. The microbial sensor can be used to assay sodium nitrite for a long period. In the same experiments the concentration of sodium nitrite was determined by both the sensor proposed and the conventional method (dime-thyl-a-naphtylamine method). A good correlation was obtained between the sodium nitrite concentrations determined by the two methods (correlation coefficient 0.99). 

Most processes for separating individual species from petroleum involve use of refined engineering methods, with distillation and selective adsorption the most important. Once separated, however, most materials then undergo chemical conversion into more desirable products. Alkylation involving propene and butenes yields C6 to C8 hydrocarbons for high-octane gasoline. Propylene becomes polypropylene, propylamine, or propylene glycol and ethers. 

More sophisticated methods involve functionalising the support before exposure to HAuCL solution. This may be achieved by incorporation of a reagent during the synthesis that produces either propylamine, or propy-lthiol groups on the surface of MCM-41145 and SBA-15.146... 

Prepn of diethanolamine dinitrate) e)Ibid,BritP 358,157 CA 26,6141(1932) [Nitration of aliphatic ammo alcohols for use as or in ezpls. For instance, dihydroxy propylamine, dipropanolamine, n-butylmono-ethanolamine, etc were nitrated by the method described in BritP 357,581(1930) CA 26,6141(1932)]... 

Ruff et al. in a series of publications described the synthesis of amine complexes of aluminum hydride [32, 33]. Their study investigated the reaction of these materials with typical Lewis bases in order to define the conditions for the stability of aluminum hydride derivatives in which the aluminum atom exhibits a coordination number of five. They first described methods for making tertiary alkyl amine complexes of aluminum hydride utilizing lithium aluminum hydride and an amine hydrochloride. A finely ground lithium aluminum hydride was placed together with trimethylammonium chloride (ratio 1 2). They prepared other trialkylamine alanes and the N-dialkylaminoalanes, in a similar fashion. These adducts of alane were found to sublime readily at temperatures up to 40 °C except for the tri-n-propylamine alane, which sublimed very slowly and could also be recrystallized from hexane at — 80 °C. 

Unsymmetrical secondary amines are readily prepared in good yields by the catalytic reduction of Schiff bases at moderate temperatures in high-or low-pressure equipment. Many examples have been cited. The intermediate imines are prepared from primary amines and aldehydes—very seldom from ketones—and may be used without isolation (cf. method 431). For the preparation of aliphatic amines, e.g., ethyl-w-propylamine and n-butylisoamylamine, a prereduced platinum oxide catalyst is preferred with alcohol as the solvent. Schiff bases from the condensation of aromatic aldehydes with either aromatic or aliphatic amines are more readily prepared and are reduced over a nickel catalyst. In this manner, a large number of N-alkylbenzylamines having halo, hydroxyl, or methoxyl groups on the nucleus have been made. Reductions by means of sodium and alcohol and lithium aluminum hydride have also been described,... 

Mishnick and co-workers have developed several techniques for determining the positions of substitutions on monosaccharide units and distribution of substituents along deriva-tized polysaccharide chains, primarily cellulose derivatives. Examples are found in references [61,62,63,64,65,66,67,68,69,70]. An important method involves perdeuteromethylation followed by partial acid-catalyzed hydrolysis, then reductive amination with propylamine, and finally permethylation to yield completely O- and A-alkylated charged oligosaccharides that are analyzed by MALDI-TOF-MS [68,70]. Statistical methods are then applied. 

The thiophosphamide ester derivatives 79 (Section III.B.l) obtained from samples spiked with standard aromatic amines and 3-phenyl-1-propylamine as internal standard were separated and determined by GC-FPD, using two capillary columns in tandem and a 526 nm filter in the optical path. The LOD (SNR 3) for aniline (la), 2-toluidine (lb), 3-toluidine (lc), 3-ethylaniline (If), 4-ethylaniline (lg), 2,3-xylidine (2a), 2,4-xylidine (2b) and 2,6-xylidine (2d) were 50, 100, 40, 30, 30, 50, 50 and 100 pg, respectively. This method was applied for analysis of smoke collected in the laboratory by burning materials as varied as chicken meat, sausage, sardine, dried squid, bread, black pepper, soy sauce, wood chips, rubber and cigarettes (main-stream and side-stream smoke). All smokes showed the presence of ppm concentrations of the eight standard aromatic amines mentioned above, but none contained detectable concentrations of all of them169. 

Benzazocines have also been synthesized using photolytic methods.243 245 For example, 112 was prepared by photochemical cyclization of A-(chloro-acetyl)-3-(3,4-dimethoxyphenyl)propylamine.243... 

Sample preparation and derivatization methods for GC analysis of BAs have been also proposed. In a method developed by Daudt and Ough (1980), amines are distilled from the alkalized grape juice or wine sample and trapped in an acidified solution. After concentration under vacuum, methylamine, dimethylamine, ethylamine, diethylamine, n-propylamine, isobutylamine, a-amylamine, isoamylamine, pyrrolidine, and 2-phenethylamine in their salt form are derivatized with triflu-oroacetic (TFA) anhydride. TFA derivatives are extracted with ethyl ether and analyzed by GC-MS with a capillary fused silica poly( ethylene) glycol (PEG) column and the following oven temperature program 8 min at 70 °C, l°C/min to 160 °C, isotherm for 90 min. 

Peculiarities of desolvation of crystallosovates of zinc(II) porphyrins with benzene, n-propylamine and their mixtures have been studied by method of thermogravimetric analysis. 

Since then most isocyanides have become readily available by the transformation (1) -> (2), the method of choice for the preparation of isocyanides. The best dehydrating agents for (1) are phosgene and diphosgene in the presence of triethylamine, and phosphorus oxychloride in the presence of diiso-propylamine. °... 

The [18]N2P4 macrocycle was prepared by a 2 2 cyclic condensation of bis(2-chloroethyl)propylamine and the dipotassium salt of l,2-bis(phen-ylphosphino)ethane in THF (method AA-4) (Ciampolini et al., 1983). 

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