693-13-0Relevant articles and documents
Process method for increasing yield of N, N '-diisopropylcarbodiimide product
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Paragraph 0019-0023, (2021/01/29)
The invention discloses a process method for improving the yield of an N, N '-diisopropylcarbodiimide product, and relates to the technical field of organic chemical synthesis, and the process methodcomprises the following steps: reacting isopropylamine and carbon disulfide by using chlorobenzene as a solvent to generate diisopropylthiourea, and carrying out suction filtration; using hydrogen peroxide as an oxidizing agent, using ethyl tert-butyl ether as a solvent, performing primary oxidation, removing hydrogen sulfideafter oxidation to generate N, N '-diisopropylcarbodiimide and sulfur; carrying out secondary oxidation, removing sulfur by using sodium hydrosulfide, washing with water, drying, evaporating out the solvent, adding potassium carbonate into the DIC crude product without thesolvent, controlling the temperature to be 55-65 DEG C, stirring for 0.3-1 hour, controlling the pressure to be less than -0.08 MPa, and distilling to obtain qualified DIC; by adding potassium carbonate, the stability of N, N '-diisopropylcarbodiimide is facilitated, and the N, N'-diisopropylcarbodiimide is prevented from being decomposed at a high temperature so that the yield is increased.
N,N'-diisopropyl carbodiimide preparation method
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Paragraph 0039-0042; 0043; 0045-0048; 0051-0054, (2019/04/06)
The invention belongs to the technical field of organic synthesis and particularly relates to an N,N'-diisopropyl carbodiimide preparation method. The method includes steps: adopting isopropylamine and carbon disulfide to synthesize N,N'-diisopropyl thiourea in a solvent; subjecting the N,N'-diisopropyl thiourea to suction filtration, drying and primary oxidization; performing secondary oxidization reaction, adding a catalyst and an oxidant, and performing reaction for 1h at 60-65 DEG C; performing desulfurizing treatment, adding sodium sulfide solution into oxidation liquid, heating to 70-75DEG C, and performing reaction for 1-2h; adding caustic soda flakes to neutralize, washing, separating a water layer, adding a drying agent for drying, evaporating out the solvent, and performing vacuum rectification to obtain N,N'-diisopropyl carbodiimide. The N,N'-diisopropyl carbodiimide preparation method has advantages that wastewater recycling can be realized, emission is avoided, and accordingly environmental pollution is avoided; simplicity in feeding and aftertreatment, low production cost, high yield and high purity are realized.
Synthesis and Characterization of Tungsten Nitrido Amido Guanidinato Complexes as Precursors for Chemical Vapor Deposition of WNxCy Thin Films
Nolan, Michelle M.,Touchton, Alexander J.,Richey, Nathaniel E.,Ghiviriga, Ion,Rocca, James R.,Abboud, Khalil A.,McElwee-White, Lisa
, p. 46 - 53 (2018/01/17)
Tungsten nitrido amido guanidinato complexes of the type WN(NR2)[(NR′)2C(NR2)]2 (R = Me, Et; R′ = iPr, Cy) were synthesized as precursors for aerosol-assisted chemical vapor deposition (AACVD) of WNxCy thin films. The reaction of tungsten nitrido amido complexes of the type WN(NR2)3 (R = Me, Et) with two equivalents of a carbodiimide R′N=C=NR′ (R′ = iPr, Cy) resulted in two insertions of a carbodiimide into W–N(amido) bonds, affording bis(guanidinato) amido nitrido tungsten complexes. These compounds were characterized by 14N NMR, indicating distinctive chemical shifts for each type of N-bound ligand. Crystallographic structure determination of WN(NMe2)[(NiPr)2C(NMe2)]2 showed the guanidinato ligands to be non-equivalent. The complex WN(NMe2)[(NiPr)2C(NMe2)]2 was demonstrated to serve as a precursor for AACVD of WNxCy thin films, resulting in featureless, X-ray amorphous thin films for growth temperatures 200–400 °C.