96-23-1Relevant articles and documents
Unconventional reactivity of epichlorohydrin in the presence of triphenylphosphine: isolation of ((1,4-dioxane-2,5-diyl)-bis-(methylene))-bis-(triphenylphosphonium) chloride
Mannu, Alberto,Di Pietro, Maria Enrica,Priola, Emanuele,Baldino, Salvatore,Sacchetti, Alessandro,Mele, Andrea
, p. 1663 - 1674 (2021)
The selective formation of the heterocyclic salt ((1,4-dioxane-2,5-diyl)-bis-(methylene))-bis-(triphenylphosphonium) chloride was observed when epichlorohydrin and triphenylphosphine were reacted in CH2Cl2 at room temperature. Slow evaporation from a mixture of ethanol and ethyl acetate allows to isolate monocrystals of the heterocyclic phosphonium salt. Mechanistic investigations point to the formation of the zwitterionic intermediate 1-chloro-3-(triphenylphosphonio)-propan-2-olate, which can dimerize and generate the 1,4-dioxane derivative. In the exclusive presence of a Br?nsted acid as HCl, which usually facilitates epoxide ring opening, the exclusive formation of 1,3-dichloro-2-propanol was although observed. Also, when epichlorohydrin, PPh3, and a stoichiometric amount of HCl were mixed, (2-chloro-3-hydroxypropyl)-triphenylphosphonium chloride was formed and its isolation in pure form provides monocrystals subjectable to X-ray analysis.
Preparation method for 1,3-propylene glycol from glycerol
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Paragraph 0066-0076, (2021/04/10)
The invention relates to a preparation method for 1,3-propylene glycol from glycerol, wherein the preparation method comprises the steps of chlorohydrination reaction, cyclization reaction, hydrogenation reaction and the like. The glycerin conversion rate of the preparation method reaches 99% or above, the yield of 1,3-propylene glycol reaches 65% or above, and the preparation method has the advantages of being simple in process, mild in reaction condition, small in investment, high in technical safety and easy to operate and control.
Preparation method of sodium beta-glycerophosphate containing crystal water
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Page/Page column 5-7, (2020/12/08)
The invention discloses a preparation method of sodium beta-glycerophosphate containing crystal water. The method comprises the following steps: A) taking epoxy chloropropane as an initial raw material, slowly dropwise adding the epoxy chloropropane into hydrochloric acid, reacting for 1-6 hours, adjusting the pH value to 3-4 by using a sodium hydroxide solution, carrying out vacuum distillation to remove moisture, distilling to 60 DEG C, adding a drying agent, stirring for 1 hour, and filtering to obtain 1, 3-dichloropropanol; B) adding the 1,3-dichloropropanol into an esterification reactionkettle, adding a phosphating agent, heating the temperature to 80-130 DEG C, controlling the temperature to esterify for 10-20 hours, after esterification is finished, adding water for dilution, dropwise adding the sodium hydroxide solution, adjusting the pH value to be 9-13, keeping the temperature at 40-80 DEG C, hydrolyzing for 3-5 hours, adding magnesium oxide or calcium oxide and stirring for 2 hours at 60-80 DEG C, adding activated carbon and stirring for 1 hour, the negative pressure distillation concentration being 70%-75%, adding ethyl alcohol, carrying out cooling and stirring and filtering to obtain the sodium beta-glycerophosphate. According to the invention, the generation of sodium alpha-glycerophosphate is avoided, and the sodium beta-glycerophosphate containing crystal water and not containing crystal water can be flexibly prepared.