- Method for preparing dichloro monoalkyl phosphine
-
The invention discloses a method for preparing dichloro monoalkyl phosphine. When sodium chloride is used for decomplexing reaction of a binary complex of dichloro monoalkyl aluminum or alkyl aluminum sesquichloride and phosphorus trichloride, alkane solvents are added, the dissociated dichloro monoalkyl phosphine enters the alkane solvents, alkane solution of the dichloro monoalkyl phosphine and newly-generated NaAlCl4 solids are filtered and separated, mixture of the product dichloro monoalkyl phosphine and the alkane solvents can be distilled and separated and can also directly enter a next application process without separation, decomposition of traditional dichloro monoalkyl phosphine in high-temperature distillation is avoided, yield is improved, and waste residues are reduced.
- -
-
Paragraph 0065-0066
(2017/08/29)
-
- Microsynthesis and electron ionization mass spectral studies of O(S)-alkyl N,N-dimethyl alkylphosphono(thiolo)thionoamidates for Chemical Weapons Convention verification
-
RATIONALE The availability of mass spectra and interpretation skills are essential for unambiguous identification of the Chemical Weapons Convention (CWC)-related chemicals. The O(S)-alkyl N,N-dimethyl alkylphosphono(thiolo) thionoamidates are included in the list of scheduled CWC-related compounds, but there are very few spectra from these compounds in the literature. This paper examines these spectra and their mass spectral fragmentation routes. METHODS The title chemicals were prepared through microsynthetic protocols and were analyzed using electron ionization mass spectrometry with gas chromatography as a MS-inlet system. Structures of fragments were confirmed using analysis of fragment ions of deuterated analogs, tandem mass spectrometry and density functional theory (DFT) calculations. RESULTS Mass spectrometric studies revealed some interesting fragmentation pathways during the ionization process, such as alkene and amine elimination and McLafferty-type rearrangements. The most important fragmentation route of the chemicals is the thiono-thiolo rearrangement. DFT calculations are used to support MS results and to reveal relative preference formation of fragment ions. The retention indices (RIs) of all the studied compounds are also reported. CONCLUSIONS Mass spectra of the synthesized compounds were investigated with the aim to enrich the Organization for the Prohibition of Chemical Weapons (OPCW) Central Analytical Database (OCAD) which may be used for detection and identification of CWC-related chemicals during on-site inspection and/or off-site analysis such as OPCW proficiency tests. Copyright
- Saeidian, Hamdollah,Babri, Mehran,Abdoli, Morteza,Sarabadani, Mansour,Ashrafi, Davood,Naseri, Mohammad Taghi
-
p. 2805 - 2814
(2013/01/15)
-
- ANHYDROUS DERIVATIVES OF ACIDS OF TRIVALENT PHOSPHORUS CONTAINING A CYANO GROUP
-
Chloro- and O-acetyl cyanides of trivalent phosphorus disproportionate into the corresponding dicyanides and dichlorides or diacyl derivatives of P(III), while S-acetyl cyanothiophosphites and -phosphonites are thermally stable.Alcoholysis of S-acetyl cyanothiophosphite at room temperature is accompanied by the formation of O.O-diethyl S-acetyl thiophosphite.At low temperature, this reaction gives diethyl cyanophosphite.
- Pudovik, A. N.,Nazmutdinova, V. N.,Chirkova, L. P.
-
p. 551 - 554
(2007/10/02)
-
- Preparation and -Cycloaddition of Methylthio-chlorophosphanes RP(Cl)SMe (R = Me, Et, Ph)
-
The methylthio-chlorophosphanes RP(Cl)SMe are prepared in good yields (62-65percent) by condensation reactions of the corresponding dichlorophosphanes RPCl2 with methanethiol in the presence of trimethylamine (molar ratio 1:1:1). 1 and 3 have been used to produce 3-phospholene sulfides in a one-pot process by reaction with 1,3-dienes at 70 to 100 deg C.Reaction proceeds via -cycloadducts, which in suitable cases can be isolated and used for the preparation of the corresponding 3-phospholene oxides.New compounds were characterized by elemental analysis and spectroscopic investigations (NMR, MS). - Keywords: Methylthio-chlorophosphanes, 3-Phospholene Sulfides and Oxides, Mass Spectra, NMR Spectra
- Apitz, Joerg,Grobe, Joseph,Le Van, Duc
-
p. 257 - 260
(2007/10/02)
-
- Process for the preparation of phenyl- and thienyl-chlorophosphane derivatives
-
Organic chlorophosphanes of the formula II STR1 in which R1 =an aromatic or heterocyclic radical and R2 =an aliphatic radical or Cl are prepared by reacting organic phosphorus oxychlorides of the formula I STR2 in which R1 and R2 have the meaning mentioned above with triphenylphosphane (C6 H5)3 P at an elevated temperature. The organic chlorophosphanes II are, in the main, intermediates in various specialized fields, such as the pharmaceuticals, plant protection, dyestuffs and polymers sectors.
- -
-
-
