52788-79-1Relevant articles and documents
Method for synthesizing diethylene glycol methyl tert-butyl ether
-
Paragraph 0022; 0023; 0024; 0025; 0026; 0027; 0028-0036, (2019/10/01)
The invention relates to a method for synthesizing diethylene glycol methyl tert-butyl ether. The method comprises the following steps: 1) an appropriate amount of diethylene glycol mono-tert-butyl ether is taken, and is added into an autoclave; 2) an appropriate amount of sodium hydroxide is added into the autoclave, and the added substances are stirred, and then are cooled to 50 DEG C; 3) a chloromethane gas is introduced into the autoclave, the temperature is controlled at 40-60 DEG C, and the pressure is maintained at 0.1-0.6 MPa; 4) a constant-temperature and constant-pressure reaction iscarried out for 2 h, the residual pressure is discharged, and the obtained reaction liquid is transferred into a separating funnel, and stands for 1 h; 5) the obtained supernatant is taken, an aromatic hydrocarbon is added, azeotropic treatment is carried out, and the obtained liquid is rectified and purified to obtain diethylene glycol methyl tert-butyl ether; 6) the obtained lower liquid is filtered and desalted, an aromatic hydrocarbon is added to the obtained filtrate, azeotropic treatment is carried out to obtain a distillate diethylene glycol ether, and the diethylene glycol ether is rectified and purified to obtain the diethylene glycol methyl tert-butyl ether; and 7) the diethylene glycol methyl tert-butyl ether obtained in step 5) and the diethylene glycol methyl tert-butyl etherobtained in step 6) are mixed to obtain the final product. The method has the advantages of scientific and reasonable design, simple and safe process, low requirements for devices, simplicity in separation, and high reaction yield.
Deamination Reactions, 41. Reactions of Aliphatic Diazonium Ions and Carbocations with Ethers
Kirmse, Wolfgang,Jansen, Ulrich
, p. 2607 - 2625 (2007/10/02)
Aliphatic diazonium ions and carbocations were generated by deacylation of appropriate nitrosoureas (1, 5, 9) in alcohol-ether mixtures or in 2-alkoxyethanols.Ethers were generally inferior to alcohols in capturing cationic intermediates.Formation of trialkyloxonium ions led to alkyl exchange or ring opening.The observed reactivity orders were n-butyl > isobutyl for the diazonium ions, allyl > sec-butyl > tert-butyl for the carbocations, methoxy > ethoxy and oxirane > oxetane > tetrahydrofuran for the ethers, indicating the predominance of steric effects.Neighboring group participation in 4-methoxy-1-butanediazonium ions (58) and 4,5-epoxy-1-pentanediazonium ions (74) was detectable but inefficient ( 20percent of cyclic oxonium ions).